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Materials Science and Engineering A xxx (2007) xxxxxx

Mechanical properties of ultra fine-grained HSLA and Ti-IF steels

J. Majta , K. Muszka
Metals Engineering and Industrial Computer Science Department, AGH University of Science and Technology, Mickiewicza 30, 30-059 Krakow, Poland
Received 16 November 2006; received in revised form 26 January 2007; accepted 30 January 2007

Abstract
To study strengthening phenomena in ultra fine structures of metals we employed the MaxStrain system to analyze the correlation between
parameters of thermomechanical processing and grain refinement of HSLA and Ti-aided interstitial free steels. The mechanical properties of the
investigated, ultra fine-grained steels are a combination of strengthening due to grain boundary, dislocation structures (dislocation arrangement,
cell structure) and solid solution. It was found that cell boundaries are more difficult to achieve in HSLA than in Ti-IF steel because of much lower
mobility of the dislocations and grain boundaries. An important result is the observation that total strain >5 does not cause any further improvement
in the mechanical properties of the investigated steels.
2007 Elsevier B.V. All rights reserved.

Keywords: Ultra fine-grained structure; Mechanical properties; HSLA; Ti-IF steel

1. Introduction as well as cooling conditions. As a result of these interac-

Nowadays, ultra fine or submicron-grained steels (below
1 m) are of interest for different branches of industry. For
example, usage in the automotive industry requires a proper
combination of the ductility and strength as well as good high
strain rate performance with a sufficient level of crash energy
absorption. The grain size controlling is one of the most attrac-
tive ways of improvement of the mechanical properties. The
yield stress, hardness, ductilebrittle transition temperature and
ductility can be significantly enhanced thanks to this strengthen-
ing mechanism. Moreover, this method seems to be especially
attractive because it does not require an expensive alloying
additions and existing production technology can be used. For
example, obtaining the ultra fine ferrite structure in low carbon
steel, in addition to the increase in mechanical properties, also
leads to a decrease in toughness and improves the weldability,
whereas in microalloyed steel it leads to an additional increase
in strength [1]. The combined effect of chemical composi-
tion and thermomechanical processing parameters determines
a formation of a microstructure which controls the mechanical
properties. Microalloyed elements (Nb, Ti) can interact with
the microstructure evolution in different ways depending on
the reheating conditions, deformation history and parameters
Corresponding author. Tel.: +48 12 6172643; fax: +48 12 6172576.
E-mail address: majta@metal.agh.edu.pl (J. Majta).
tions, an evolution of dislocation structure and finally diverse
refinement of the microstructure are achieved. The condition
of grain boundaries and dislocation structures directly deter-
mines the mechanical properties of deformed material. Recently
developed severe plastic deformation (SPD) techniques have
made it possible to produce submicron/nanostructures in ultra
fine-grained steels. In present work the MaxStrain system is
employed to produce submicron steel structures and to study the
effect of the processing parameters on the mechanical behavior
of such materials.
2. Experimental procedures
The goal of the experiments was to produce ultra fine-grained
structures (grain size below 1 m) and to study the mechanical
behavior of such materials as a function of different thermo-
mechanical processing. The basic chemical compositions of the
investigated steels are presented in Table 1.
In order to develop the ultra fine-grained structures, the
MaxStrain system was used. The principles of this system are
described in details in literature [2]. Distinct from most severe
plastic deformation methods, the MaxStrain technology uses
deformation in two axes while fully restraining the third axis.
The deformation process was carried out according to the
schedules summarized in Table 2. Both of the investigated steels
were tested with the same thermomechanical schedules. During

0921-5093/$ see front matter 2007 Elsevier B.V. All rights reserved.
doi:10.1016/j.msea.2007.01.135

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Table 1
Basic chemical composition of investigated steels
Steel C (wt%) Mn (wt%) Si (wt%) Al (wt%) Ti (wt%) Nb (wt%)

Ti-IF (IF) 0.0022 0.11 0.009 0.037 0.073

HSLA (Y) 0.07 1.1 0.27 0.02 0.031 0.067

Fig. 1. Examples of data collected during MaxStrain tests.

Fig. 2. Schematic representation of experimental procedure.

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the test, a part of the sample (10 mm in length) is compressed

Cooling rate,
CR2 ( C/s)
by two synchronized anvils to maintain its integrity. The sam-
ple is rotated by 90 between the consecutive deformations, and
it is restrained at the ends requiring the lateral deformation in

4
the deformation zone. In this way, a total strain of 20 can be

Total equivalent
accumulated in the structure causing substantial grain refine-
ment. Fig. 1 shows examples of temperature versus time and
strain, 2
force versus stroke data collected during tests. In the present
study, total strains of 5, 10 and 20 were applied (strain of 0.5 per




5
each pass). To study the influence of grain refinement (by SPD)
Deformation temperature,

on microstructure evolution and mechanical properties, samples

were cut in half (in longitudinal direction) and polished. Sub-
sequently, on one half of each deformed sample, TEM analysis
and the Vickers hardness tests (HV5) were carried out. The sec-
Second cycle

ond half was use to prepare the tensile samples, and tensile tests
TD2 ( C)

at room temperature with frame rate of 2 mm/min using Instron

500

4502 testing machine were performed (Fig. 2).

Cooling rate,
CR1 ( C/s)

3. Results

In the present analysis, the application of the MaxStrain

4
4
4

system makes it possible to evaluate the influence of severe

Annealing time,

deformation on microstructure refinement and, in consequence,

on mechanical properties. However, it should be emphasized,
that samples obtained in such a test are characterized by high
tA (s)

1200
1200

1200

inhomogeneity of the microstructure in the deformation zone.

Many of the already published observations have shown that
the number of high angle boundaries formed across a grain
temperature, TR /TA ( C)

depends on the crystal orientation. When the effective strain

Reheating/annealing

increases, the misorientation angle across deformation induced

dislocation boundaries increases and typical cell block structures
start to reorient into lamellar structure (Fig. 3a). However, after
annealing these dislocation structures undergo some rearrange-

500
500

500

ment, and a more stable deformation microstructure is observed

(Fig. 3b). In the present study, for example, in the case of IF2
Total equivalent.

and IF3 samples (Figs. 3b and 4) the deformation induced ultra

fine structure (nanostructured material) turned into ultra fine
strain, 1

grains (nanocrystalline material) by the aid of recovery during

annealing at 500 C (continuous recrystallization).
5
5
20
5
5

Fig. 5 presents TEM micrographs of ferrite in the deformed

and annealed HSLA steel. After the compression test with a total
strain of 5, the ferrite microstructure mainly consisted of parallel
time, tR (s)
Reheating

bands of elongated grains having a width of 0.31 m. This is

a typical microstructure subdivided by lamellar boundaries. In



300

some areas of the sample, the increase in boundary spacing is

Deformation temperature,

observed. Inside the band interior, dislocation cell boundaries

can be found. However, the dislocation density inside each cell is
relatively low. The microstructure after deformation with a total
MaxStrain deformation schedules

strain of 20 and annealing is shown in Fig. 5b. Very fine equiaxed

grains with an average grain size of 0.3 m were formed in this
First cycle

TD1 ( C)

specimen. Fig. 5c shows a TEM micrograph of the sample after

20
20
20
500
20

deformation with a total strain of 10 (schedule Y5). In this case

the cell structure is not as refined and the boundaries appear
Sample symbol

to be blurred. The cell size varies between 0.52 m and the

dislocation network within the cells can be observed (Fig. 5c).
Y1; IF1
Y2; IF2
Y3; IF3
Y4; IF4
Y5; IF5
Table 2

As it is discussed elsewhere [3] the degree of the microstructural

inhomogeneities including deformation bands, slip bands and

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Fig. 3. TEM (bright-field) micrographs of deformed and annealed samples of IF1 (a) and IF2 (b).
microshear bands is higher in fine grains than in coarse one at the
same level of strain. The steels investigated in the present study
show significantly different grain sizes, i.e. 100 and 12 m in
the case of IF-Ti and HSLA steel, respectively. Additionally, the
presence of fine Nb-precipitates and solid solution strengthening
affect the dislocation movement in microalloyed steels. Hence,
the microstructures of HSLA steel are more inhomogeneous than
in Ti-IF steel, as can be seen in Fig. 5.
Fig. 4. Cell structure in deformed and annealed IF3 sample.
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It can be noticed that the principal effect of annealing on the
dislocation structure is the development of a more pronounced
delineation of the cell walls. Additionally, as it was stated
elsewhere [4], during the early stage of annealing the free dis-
locations inside the cells are being attracted by the dislocations
located in the tangled cell wall. In the meantime, dislocations
in the cell wall probably undergo some slight rearrangement.
It is believed that these effects evolve a relaxation of the long-
range stress field and finally is responsible for the disturbances
of flow stress which have been observed. The dislocation struc-
ture is also dependent on the strain rate [5,6]. The strain rate
affects both the short-range and long-range stress [7]. However,
it is found in the present study that applied additional deforma-
tion after annealing (schedule Y5) significantly decreases these
effects and additionally, an ultra fine inhomogeneous deforma-
tion microstructure is observed in this case.
In the mechanical propertiesmicrostructure relationships,
the strength contribution of low-angle dislocation boundaries
is generally related to the reciprocal boundary spacing or to the
dislocation content in the boundaries. The grain size dependence
of yield stress is well known as the so-called HallPetch rela-
tion and has been widely used to predict both, yield stress and
flow stress of the materials. However, there are some reports
suggesting that this relation is no longer of effective use for
the description of the deformation process of materials with
submicron/nanostructure. It is still unclear how deep into the
nano-scale regime the HallPetch relation can be expected to
continue. Some authors suggest that for crystalline materials
there should be a maximum strength at a critical grain size [1,8].
When the grain size is lower than a critical value, an inverse
HallPetch relation is observedflow stress decreases with
decreasing grain size. As grain sizes are reduced to the nano-
scale regime, the percentage of grain boundary atoms increases
correspondingly. To evaluate the influence of the thermomechan-
ical treatment on the dislocation substructure and the mechanical
properties of the analyzed materials, tensile tests were carried
out on deformed specimens. Comparing the flow curves obtained
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Fig. 5. TEM (bright-field) micrographs of deformed and annealed samples of Y1 (a), Y3 (b) and Y5 (c).

in the tensile tests and hardness measurements it can be seen

that because of the applied annealing the ductility of the ultra
fine-grained steels can be improved significantly. However, it
is important to mention that strong mechanical inhomogeneity
is observed in the deformation zone (see Fig. 6). The tensile
test results indicate that the history of the thermomechanical
treatment has significant influence on the mechanical response
of the final material (Fig. 7). In addition, in the range of very
high deformations similar strain-stress curves for significantly
different total strain values can be observed (IF1 and IF3). It
should be noted that in the case of sample IF3, the microstruc-
ture was recovered. However, the gain in the form of ductility is
small. For the Ti-IF steel, the flow stress increases by increasing
applied total strain but the uniform elongation is not controlled
by the structure refinement. These behaviors show a possible
way as how to obtain a good balance of strength and ductil-
Fig. 7. Engineering stressstrain curves for studied samples.
ity in the ultra fine-grained Ti-IF steel. In the case of HSLA

steel the situation is more complex. As can be seen in Fig. 7

the specimens of steel HSLA show extremely high strength in
comparison to the Ti-IF steel for similar schedules of deforma-
tion. Also the yield ratio (YS/TS) is high in ultra fine-grained
HSLA steel (Table 3). The reasons for these effects are attributed
to microalloyed elements (Nb, Ti), which can interact with the

Table 3
Mechanical properties after deformation (schedules are shown in Table 2)
Sample YS (MPa) TS (MPa) YS/TS HV5

IF1 366 610 0.6 201

IF2 304 526 0.58 178
IF3 360 597 0.6 193
IF4 364 488 0.75 188
IF5 454 546 0.83 185
Y1 700 912 0.77 309
Y2 436 862 0.51 321
Y3 850 984 0.86 354
Fig. 6. Normalized hardness distributions in samples after MaxStrain deforma- Y4 424 928 0.46 301
tion. HV5c , hardness in the centre of each sample; HV5x , the current hardness Y5 488 1045 0.47 333
value at the distance x from the centre in the longitudinal and transversal direc-
tion. YS, yield strength; TS, tensile strength; HV5, Vickers hardness.

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microstructure evolution in solution or as a very fine precipi-
tate of Nb(C,N). Further investigations are required to clarify
the physical mechanisms and their interactions because of the
retardation of dislocation movements and cell structure forma-
tion in the microalloyed steels. These effects play an important
role not only during heavy deformation (plastic flow, evolution
of strengthening mechanisms, fracture initiations) but also in the
subsequent annealing process.
4. Conclusions
The evolution of ultra fine-grained HSLA and Ti-IF steels
were studied in MaxStrain multi-compression tests with total
strain of 5, 10 and 20. Ultra fine ferrite grains with an average
diameter of 0.3 and 0.8 m were obtained in HSLA and Ti-IF
steel, respectively. Present results support earlier observations
that cells formed in Ti-IF steel are more sharply defined but
larger than cells formed in HSLA steel. Results of experimen-
tal measurements of the cell diameter will be employed in the
model of flow stress and yield strength [9]. It is presented that
by studying the correlation between parameters of thermome-
chanical processing and dislocation structures the mechanical
behavior of ultra fine-grained steels can be controlled. Mechan-
ical property test data confirmed a significant increase in strength
and hardness by refinement of ferrite structure. Besides, the
ductility of the investigated steels can be improved thanks to
the application of the annealing, which turns the deformation
induced substructure into stable ultra fine grains.
On the basis of the presented work, main conclusions can be
formulated as follows:
Please cite this article in press as: J. Majta, K. Muszka, Mater. Sci. Eng. A (2007), doi:10.1016/j.msea.2007.01.135
1. Total strain > 5 does not cause any further improvement in
the mechanical properties.
2. The cold deformation process with subsequent annealing at
500 C can be replaced by deformation at 500 C.
3. From the point of view of the final product implementation,
comparing Ti-IF and HSLA steels, significant differences in
the final properties occur in the deformation schemes No. 2
and 5.
Acknowledgement
Financial assistance from the Polish Committee for Scien-
tific Research (Poland, Research Grant No. 3T08B 042 27) is
gratefully acknowledged.
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