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Materials Science and Engineering A 523 (2009) 173177

Contents lists available at ScienceDirect

Materials Science and Engineering A

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

Small-scale mechanical property characterization of ferrite formed during

deformation of super-cooled austenite by nanoindentation
Tae-Hong Ahn a , Kyung-Keun Um b , Jong-Kyo Choi b , Do Hyun Kim a , Kyu Hwan Oh a ,
Miyoung Kim a , Heung Nam Han a,
a
b

Department of Materials Science and Engineering, Seoul National University, San 56-1, Shinrim-dong, Kwanak-gu, Seoul, 151-744, Republic of Korea
Plate Research Group, POSCO Technical Research Laboratories, Goedong-dong 1, Nam-gu, Pohang, 790-785, Republic of Korea

a r t i c l e

i n f o

Article history:
Received 20 February 2009
Received in revised form 23 May 2009
Accepted 25 May 2009

Keywords:
Ultrane-grained microstructure
Dynamic transformation
Phase transformation
Nanoindentation
Mechanical properties
Hardness

a b s t r a c t
The mechanical properties of dynamically and statically transformed ferrites were analyzed using a
nanoindentater-EBSD (Electron BackScattered Diffraction) correlation technique, which can distinguish
indenting positions according to the grains in the specimen. The dilatometry and the band slope and contrast maps by EBSD were used to evaluate the volume fractions of two kinds of ferrite and pearlite. Fine
ferrites induced by a dynamic transformation had higher nano-hardness than the statically transformed
coarse ferrites. Transmission electron microscopy (TEM) showed the dynamic ferrites to have a higher
dislocation density than the statically transformed ferrites.
Crown Copyright 2009 Published by Elsevier B.V. All rights reserved.

1. Introduction
Recently, there has been increasing demand for the manufacture
of ultrane-grained ferritic steels to satisfy the increasing demand
for structural steels with improved strength and toughness [19].
The key technology for producing ultrane-grained ferritic steels is
to impose heavy deformation to super-cooled austenite to induce
a dynamic formation of ferrite grains [10]. The Strain-Induced
Dynamic Transformation (SIDT) of super-cooled austenite has been
highlighted as a process that can overcome the limitations of
conventional ThermoMechanical Control Processing (TMCP). Both
dynamically and statically transformed ferrites coexist in SIDTed
steels due to the lower volume fraction of SIDTed ferrite in low carbon steel than the equilibrium ferrite fraction at a given processing
temperature [5,7,10].
It is known that the grain size of the dynamic ferrite is ner
than that of static one [5]. Since the strength of the ne-grained
steel has been described by the Hall-Petch relationship, which is
taken the interaction between grain boundary and dislocation into
account, the amount and the grain size of dynamic ferrite are very
important in achieving the higher strength and toughness of the
steel. However, this strength evaluation from the Hall-Petch rela-

Corresponding author. Tel.: +82 2 880 9240; fax: +82 2 872 8785.
E-mail address: hnhan@snu.ac.kr (H.N. Han).

tionship is not based on the mechanical property itself of the inside

of ferrite grain. On the contrary, there might be a possibility that
ne dynamic ferrites could show the softer mechanical behavior
because this dynamic ferrite transforms at higher temperature than
static one. In order to compare the small-scale mechanical characteristics of each ferrite itself by grains, a nanoindentation would be
a good candidate.
In this study, quantitative dilatometric analysis was used to
determine the volume fractions of dynamic and static ferrite in low
carbon steel during deformation and subsequent cooling, respectively. The small-scale mechanical properties of the two types of
ferrite were characterized by nanoindentation. A nanoindentaterEBSD (Electron Backscatter Diffraction) correlation technique was
used to distinguish the indenting positions according to the grains
in the specimen. TEM observations of the dislocation densities
showed a difference in nano-hardness between the two types of
ferrite.
2. Experimental
The composition of steel used in this study was
Fe0.1C1.5Mn0.25Si0.05V0.01Ti0.04Nb0.0036N
(wt.%).
The Ae3 temperature of this steel was estimated to be 810 C
under the para-equilibrium condition using Thermo-Calc [11]. A
vacuum induction melted ingot was soaked and hot-rolled to a
15 mm thick plate at temperatures between 1000 and 1200 C.

0921-5093/$ see front matter. Crown Copyright 2009 Published by Elsevier B.V. All rights reserved.
doi:10.1016/j.msea.2009.05.050

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Fig. 1. Comparison of relative dilatation curves between deformed (SIDT) and undeformed specimens during cooling at the rate of 2 C/s.

Cylindrical specimens, 10 mm in diameter and 15 mm in height,

were machined from those plates for thermo-mechanical processing on a Gleeble 3800. The specimens were reheated to
1200 C for 5 min resulting in an austenite grain size of 77 m.
The specimens were then cooled to 720 C at a rate of 2 C/s, and
deformed immediately with upto 70% compression at a constant
strain rate of 1.0/s. The deformation temperature was chosen to
be 20 C above the Ar3 temperature of 700 C. After deformation,
the specimens were cooled immediately to room temperature at
2 C/s. The dilatometric change in the diametrical direction in the
middle of the specimens was measured over the entire process,
including heating, deformation and cooling.
After thermo-mechanical processing, sample preparation for
nanoindentation was performed by mechanical grinding using a
diamond suspension and chemical etching with 3% nital solution to
expose clearly the grain boundary by SPM (Scanning Probe Microscope) equipped in the nanoindenter. The nano-hardness of the
dynamically and statically transformed ferrites was measured using
a Hysitron Tribolab nanoindenter. Total 37 indentations were carried out inside grains one by one. The maximum load for each indent
was 800 N. The grains could be classied into dynamic and static
ferrite by measuring the grain size in the EBSD image.
An EBSD (HKL Nordlys Channel 5) system was used to measure
the crystallographic orientation and size of each ferrite grain. A total
area of 1400 1000 pixels was indexed with a step size of 0.1 m.
The indentation positions were determined by the grains using both
EBSD and SPM image. In addition, the dislocation densities in the
dynamically- and statically-transformed ferrites were observed by
TEM (Tecnai F20). Thin foils were prepared for the TEM observation
by mechanical polishing and electropolishing with a solution containing 10% perchloric acid and 90% methanol followed by Ar+ ion
milling to remove the oxidized or contaminated surface layer.
3. Results and discussion
The austenite remaining in the specimen that is subject to immediate cooling to room temperature after deformation at above the
Ar3 temperature and below the Ae3 temperature undergoes a static
austenite-to-ferrite and austenite-to-pearlite transformation. The
volume fraction of the statically transformed phase after SIDT could
be evaluated by a comparison with the relative dilatation curve
during continuous cooling of the specimen without deformation.
Fig. 1 shows the relative dilatation curves for both the deformed
and undeformed samples during cooling at 2 C/s. The volume fraction of the statically transformed phase, fS , in the SIDTed specimen
was determined by applying the lever rule [1217] to the dilatation

Fig. 2. (a) Grain size map measured by EBSD for the specimen undergone SIDT,
(b) band contrast and slope combined map for classifying pearlite and (c) image
of microstructure classied into the dynamically and statically transformed ferrites
and the pearlite.

curves. For the lever rule, the dilatations curve of the undeformed
specimen was used as the linear segment in the single austenite
region. The relative dilatometric curve was used to compensate for
large changes in the length of the dilatometric specimen due to the
heavy compressive deformation. The volume fraction of dynamic
ferrite, fD , was obtained from the equation, fT = fS + fD , where fT is
the volume fraction of the total transformed phase. In this case,
the volume fractions of dynamic ferrite and the static phase were
determined to be 0.48 and 0.52, respectively. The volume fraction
of the statically-transformed pearlite after SIDT was determined to
be approximately 0.1 from optical microscopy and the combined
band contrast and slope map [18] obtained from EBSD, as shown in
Fig. 2(b). Therefore, the volume fraction of static ferrite is 0.42.

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175

Fig. 3. (a) Band contrast image measured by EBSD after indentations conducted, (b) SPM images with indentation marks: red, blue and black circles indicate the dynamically
and statically transformed ferrite and the pearlite, respectively, and (c) loaddisplacement curves for the clear indents, which exist inside a grain (For interpretation of the
references to color in this gure legend, the reader is referred to the web version of the article)

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T.-H. Ahn et al. / Materials Science and Engineering A 523 (2009) 173177

Fig. 4. Bright eld images obtained by TEM for (a) dynamically and (b) statically transformed ferrites.

Fig. 2(a) shows the grain size map of the SIDTed specimen
measured by EBSD. The fraction of well-indexed pixels was approximately 96%, and the un-indexed pixels around grain boundaries
were lled by extrapolation using the information of the adjacent
pixels. The grain boundaries were dened as high angle ones with
a misorientation angle >15 . As shown in this gure, two types
of ferrite grain can be observed: very ne ferrite grains formed
near the prior austenite grain boundaries and coarse ferrite grains
in the prior austenite grains. The dynamically transformed ferrite
grains were much ner than the statically transformed grains. This
bimodal grain size distribution in the ferrite phase might make
it possible to classify the dynamically and statically transformed
ferrite. The critical grain size was estimated to be 5.7 m, which corresponds to a volume fraction of 0.48 for dynamic ferrite based on
the dilatometry results in Fig. 1. The statically transformed pearlite
after SIDT was classied from the band contrast and slope combined
map [18], as shown in Fig. 2(b). An image of the microstructure classied into the dynamically- and statically-transformed ferrite, and
the statically-transformed pearlite was obtained from the criterion
of grain size, as shown in Fig. 2(c).
Nanoindentation was used to compare the small-scale mechanical properties of the two types of ferrite. The nanoindentater-EBSD
correlation technique was suggested due to the difculty in classifying grains, i.e. dynamic and static ferrites and pearlite, using
SPM only. Fig. 3(a) shows a band contrast image by EBSD. As shown
in this gure, two types of ferrite grain can be well classied.
In ve blue marked regions, the indentations were performed as
shown in Fig. 3(b). Among the indentation points, only the clear
indents inside a grain were selected and classied into dynamic and
static ferrites based on the criterion of grain size. Fig. 3(c) shows
their loaddisplacement curves. The mean nano-hardness of the
dynamic and static ferrites was 3.71 0.11 GPa and 3.23 0.02 GPa,
respectively. The nano-hardness of pearlite was much higher than
those of the ferrites.

The dynamic ferrite was approximately 15% harder than the

static ferrite. This is in contrast to the reports showing that the
transformation temperature of dynamic ferrite is higher than that
of static ferrite. There are some reports showing that supersaturated
carbon in dynamic ferrite forms very small cementite particles on
the ferrite boundary [10,19]. This supersaturated carbon in dynamic
ferrite is expected to be a strengthening mechanism. In addition, the
plastic deformation occurring after SIDT might increase the dislocation density in dynamic ferrite. A large number of TEM observations
of the inside of the grains were made to conrm the difference in
dislocation density between the two types of ferrite grains. The dislocation density was calculated from about 40 observed images for
each ferrite grains. Fig. 4 shows typical TEM images of the two types
of ferrite grains that contain dislocation structures. The average
dislocation densities of the dynamic and static transformed were
2.7 1014 m2 and 8.7 1013 m2 , respectively. A higher density of
dislocations of dynamic ferrite is due to work-hardening after SIDT.
The higher dislocation density may also be one of the strengthening mechanisms of dynamic ferrite. This difference in dislocation
density between the two types of ferrites may be used to help distinguish them from a microstructural analysis based on another
EBSD technique, such as a local misorientation map or grain average
misorientation.
4. Conclusion
In conclusion, this study examined the nanoindention properties of ne-grained ferrite transformed dynamically by heavy
deformation using a nanoindentater-EBSD correlation technique,
which can distinguish the indenting positions according to the
grains in the specimen. The critical grain size for classifying the
dynamically and statically transformed ferrites was determined
by dilatometry analysis. In addition, the volume fraction of the
statically-transformed pearlite after SIDT could be determined

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T.-H. Ahn et al. / Materials Science and Engineering A 523 (2009) 173177

from the combined band contrast and slope map from EBSD. The
ne ferrites induced by the dynamic transformation had higher
nano-hardness than the static ones. Overall, ne dynamicallytransformed ferrite grains have a higher dislocation density than
statically transformed ferrite grains.
Acknowledgement
This work was supported by the Korea Science and Engineering
Foundation (KOSEF) grant funded by the Korea government (MOST)
(R0A-2007-000-10014-0). Drs. Um and Choi would like to thank for
the support by one of National mid-term key technology projects
(10028396-2008-13).
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