Author’s Accepted Manuscript

Effect of 10% ausforming on impact toughness of

nano bainite austempered at 300°C

Sahand Golchin, Behzad Avishan, Sasan Yazdani

www.elsevier.com/locate/msea

PII: S0921-5093(16)30025-9
DOI: http://dx.doi.org/10.1016/j.msea.2016.01.025
Reference: MSA33212
To appear in: Materials Science & Engineering A
Received date: 25 October 2015
Revised date: 22 November 2015
Accepted date: 7 January 2016
Cite this article as: Sahand Golchin, Behzad Avishan and Sasan Yazdani, Effect
of 10% ausforming on impact toughness of nano bainite austempered at 300°C,
Materials Science & Engineering A,
http://dx.doi.org/10.1016/j.msea.2016.01.025
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 Effect of 10% ausforming on impact toughness of nano bainite
austempered at 300 °C
Sahand Golchina, Behzad Avishan*b, Sasan Yazdania
a
Faculty of Materials Engineering, Sahand University of Technology, Tabriz, Iran.
b
Department of Materials Engineering, Azarbaijan Shahid Madani University, Tabriz, Iran.

*Corresponding author: avishan@azaruniv.edu

Abstract

The volume fraction and morphology of the microstructural constituents are extremely important
when discussing the impact toughness of nanostructured bainitic steels. On the other hand,
microstructural features can be influenced by plastic deformation of austenite prior to isothermal
bainitic transformation. This article aims to investigate the effect of 10% ausforming process
before austempering heat treatment on impact toughness of nanostructured low temperature
bainitic steels austempered at 300 °C. Results indicate that the volume fraction and morphology
of high carbon retained austenite within the microstructure are important factors affecting the
impact toughness energy. However results showed that the role of bainitic sheaves cannot be
ignored due to their valuable effect of arresting/deflecting the cracks. It has been found that
bainitic sheaves grow at more limited crystallographic variants in ausformed samples which can
influence the value of the impact energy absorbed during straining the samples.

Keywords: Nano bainite; Ausforming; Impact toughness; X-ray diffraction.

1. Introduction

It is well known that almost 1.5 Wt.% Si addition can retard the cementite precipitation in
bainitic steels. This, results in a microstructure composed of bainitic ferrites and retained
austenite which can remain stable at room temperature due to its high C content and therefore
low Ms temperature. Consequently, replacing brittle interlath cementite by ductile interlath films
of retained austenite can increase the toughness in this group of steels. However, toughness can
further be increased by refining the microstructure. A new group of these steels known as
nanostructured low temperature carbide free bainitic steels have been introduced with
distinguishable mechanical properties combinations [1-10].

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These microstructures can be obtained through a simple isothermal heat treatment procedure in a
very low temperature above the Ms temperature of steel. Nanoscale structure is being produced
in which the bainitic ferrite plates of less than 100 nm thicknesses are the main factor controlling
the strength properties, while ductility is mainly controlled by retained austenite [11-18].
Austenite is present within the microstructure in two filmy and blocky morphologies. The former
separates bainitic subunits with almost identical thicknesses with same crystallographic
orientation, aggregates of which are known as sheaves, and later spreading between sheaves of
bainite.

There are different factors deteriorating impact toughness in nanostructured bainitic steels such
as presence of coalesced bainite or microstructural bandings during dendritic solidification [19].
Presence of brittle martensite is another major reason which must be considered carefully. On the
other hand, austenite blocks are thermally and mechanically less stable because of their lower C
content especially in center regions which makes them prone to transform to martensite during
cooling to room temperature or earlier stages of deformation. So, it is essential to replace
austenite blocks with austenite films as much as possible in order to obtain superior toughness
properties. Increasing the volume fraction of bainite and therefore primary austenite
decomposition is a useful way in this regard. It is well known that bainitic transformation starts
by paraequilibrium nucleation of bainitic ferrites and progresses by their shear growth [20].
Transformation stops when the C content of the austenite reaches the value predicted by Tₒ
diagram [20-24]. Higher amount of bainitic ferrites can be achieved by decreasing the mean C
content of steel at a constant transformation temperature based on lever rule [25]. However C is
the main alloying element being added to suppress the Ms and Bs temperatures in order to be able
to conduct the bainitic transformation at lower temperatures to gain nanoscale morphology.
Besides, C increases the strength of the austenite which in turn restricts the ferrite/austenite
glissile interface motion resulting in thinner bainitic ferrite. Refining primary austenite grains
can also be effective in increasing the volume fraction of the bainitic ferrites bearing in mind that
grain boundaries are potential nucleation sites higher density of which results in higher
nucleation rate [11, 26]. Another theory is to conduct ausforming processes prior to isothermal
bainitic heat treatment in order to increase the amount of bainite present within the
microstructure [27, 28].

There are different studies investigating the bainitic transformation response to applied stress and
to ausforming process. Shipway and Bhadeshia [29] showed that compressive stresses even
lower than the yield strength of austenite could accelerate the bainitic transformation. Similarly,
it has been declared by Matsuzaki et al. [30] that bainitic transformation kinetic accelerated by
applying the uniaxial stress and higher volume fraction of bainite formed in which sheaves were
grown in favored orientations. Hu et al. [27] investigated the effect of ausforming on the bainitic
transformation in carbide free super bainitic steels. They have reported that the transformation
rate depended on ausforming temperature, nucleation rate of bainitic ferrites and growth rate of
bainitic sheaves. Meanwhile, it has been shown that there was a critical strain bellow which the

2
volume fraction of bainite and austenite were increased while conducting the ausforming above
the critical value decreased the amount of these phases. Huang et al. [31] indicated that bainitic
transformation enhanced by prior compressive deformation of retained austenite. While the
acceleration of bainitic transformation has also been approved by Freiwilling et al. [32] and Jin et
al. [33], Shirzadi et al. [34] stated that ausforming before isothermal bainitic transformation at
300 °C never accelerated the reaction. Yang et al. [35] and Laren and Yang [36] showed that
mechanical stabilization of austenite at higher amount of plastic deformation of retained
austenite during the ausforming process retarded the bainite transformation and hindered further
progress of the bainite formation. This idea was claimed before either by Shipway and Bhadeshia
[37]. Zhang et al. [38] investigated the effect of ausforming strain and temperature on bainite
formation in a medium carbon steel in which it has been reported to be possible to decrease the
Ms temperature substantially and therefore to obtain nano bainite. He et al. [39] studied the
effect of warm rolling process on kinetic of the nanostructured bainite. They have declared that
nano bainite formation was accelerated due to the prior deformation of austenite and noticeable
decrease of the incubation time was reported for samples austempered at 230 °C. Also, they have
shown that there was a slight change in the volume fraction of the retained austenite after
ausforming process where acceptable strength and elongation could be achieved. In a similar
work recently by He et al. [40], it has been suggested that multi step ausforming of nano bainite
accelerated the bainite reaction. They also reported that UTS of 2154 Mpa and total elongation of
13% could be obtained by transforming at 300 °C after 2 h in ausformed samples.

Although Shirzadi et al. [34] reported that ausforming followed by Isothermal bainitic
transformation at 300 °C could not be able to assist the variant selection occurrence, but recently
Gong et al. [28, 41] studied the microstructural variations in nanostructured bainitic steels
emphasizing on variant selection and transformation rate changes at different ausforming
processes. It has been demonstrated that ausforming prior to austempering heat treatment
increased the bainite nucleation sites and so increased the transformation rate. Moreover, strong
variant selection has been defined in that study. This article aims to study how these
microstructural changes can affect the impact toughness properties bearing in mind that
microstructural characteristics are of considerable importance during evaluating the impact
energy absorbed in material. In this regard, 10% of ausforming conducted just before bainite
transformation in a nanostructured bainite austempered at low temperature of 300 °C and impact
property has been evaluated.

2. Experimental procedure

Steel was cast in a 3000 Hz induction furnace under inert Ar atmosphere and finally electro slag
remelted through a 30% CaF2 + 70% Al2O3 reactive slag using 1300-1400 A and 24- 28 V in
order to achieve a clean material. The final chemical composition was 0.94C- 1.4Si- 2.4Ni-
1.07Al- 0.34Mo- 1.18Cr- 1.68Co- 0.9Mn- 0.1V, all in Wt.%., in which C was the main alloying

3
element being added to suppress the Ms and Bs temperatures and Si addition was essential to
retard cementite precipitation. Theoretically designed chemical composition was the result of the
phase transformation theory described elsewhere [20]. Steel was homogenized at 1200 °C after
which hot rolled to attain billet of almost 15 mm thickness. Two sets of 654015 mm3 samples
were cut and prepared from billet. Nanostructured bainite achieved in both sets based on the heat
treatment procedures illustrated in Fig. 1. Both sets of samples were austenitized at 950 °C for 30
min after which first set immediately quenched to an austempering bath of 300 °C keeping for
different austempering times. 10% thickness reduction at 300 °C were conducted by rolling the
second set of samples after which they were quenched in same austempering bath for similar
austempering times. The temperature was controlled using a thermocouple during the ausforming
process. A type K (chromel-alumel) thermocouple was attached centrally to the lateral surface of
the samples and the measured temperature variations were almost 3 °C.

Fig. 1. Schematic diagram of a) simple isothermal heat treatment and b) ausforming + isothermal
heat treatment processes of samples.

Microstructural evaluations were conducted on an OLYMPUS PMG3™ optical microscope and

MIRA3 TESCAN™ field emission gun scanning electron microscope after grinding and
polishing the samples following the standard procedure. High magnification FE-SEM
micrographs were used for ferrite plate thickness measurements using line intercept method [18,
42] in a direction normal to the plate length. Reported values are average of almost 200
measurements. Quantitative X-ray diffraction analysis was performed on a Brucker-Axs D8
Advance™ X-Ray diffractometer with monochromated CuKα, radiation at 40 kV and 40 mA. X-
ray profile refinements were used to determine the volume fraction of retained austenite using
the integrated intensities of (200), (220) and (311) austenite peaks, and those of (200), (211) and
(220) peaks of ferrite [43]. Using this number of peaks avoids possible bias due to
crystallographic texture [44]. The orientation of the bainitic sheaves were evaluated relative to
the rolling direction in optical micrographs according to the method proposed by Hase et al. [45]
by almost 150- 200 orientation measurements.

4
Charpy impact tests were conducted on 10×10×55 mm3 notched samples at room temperature.
At least 5 samples were tested at each austempering time and the average values were reported in
each test condition. Fracture surfaces of the impact samples were analyzed on same scanning
electron microscope. Finally hardness was measured as HV (30 kg) and the presented results
correspond to an average of at least 3 values.

3. Results and discussions

Fig. 2 illustrates the micrographs of non-ausformed and ausformed samples austempered at

similar austempering times. It is clear that in each set of samples, the volume fraction of the
bainite formed at 300 °C is increasing with increasing the austempering time. At earlier stages,
the amount of the bainite is much lower and microstructure consists of bainitic sheaves (dark
features), which are aggregates of parallel bainitic subunits and austenite films, separated by
blocky austenite/martensite regions (light features). Bainite transformation progresses by
increasing the austempering time and more bainitic sheaves form within the microstructure. On
the other hand, it is evident that ausforming accelerates the bainite transformation and a higher
volume fraction of bainite forms at identical austempering times. This is more evident when
comparing steels after austempering for 2h. A similar trend has been reported before [28] where
it has been shown that, desired amount of thermo mechanical processes before isothermal bainite
heat treatment increases the dislocation and stacking fault densities and consequently nucleation
and transformation rate both enhanced.

Comparing optical micrographs in both sets of samples reveals that bainitic sheaves tend to grow
in limited crystallographic directions in ausformed samples whereas sheaves in non-ausformed
specimens are grown in many different crystallographic directions. This has been quantified for
example in Fig. 3 for samples austempered for 6 and 16 h in which the bainitic sheaves’
alignments were analyzed with respect to the rolling direction in heat treated materials. It is clear
that there is a greater degree of microstructural alignment in ausformed samples comparing to
that of non-ausformed specimens. According to Gong et al. [28, 41], this is the direct
consequence of the dislocation arrays arrangement after ausforming due to which ferrite plates
and austenite films are aligned in limited directions in each austenite grain. Precise TEM and
EBSD studies by Gong et al. [28] approved that planer dislocations on active slip planes assisted
the bainite transformation and resulted in strong variant selection in nanobainite. Because the
inhomogeneous plastic flow of the individual austenite grains results in different operating slip
systems for each grain. Therefore, bainitic sheaves would be aligned along one, two or three
directions in austenite grains. Furthermore, micrographs in Fig. 2 reveal that ausforming results
in some shorter bainitic sheaves besides those long sheaves similar to the case of non-ausformed
set of samples. This has been shown to be caused by nucleation of bainitic subunits not only on
grain boundaries, but also at the interface between austenite and bainitic ferrite [28]. So far the
growth of these types is hindered by preexisting ferrite plates or dislocations which can be result

5
in shorter bainitic sheaves. Finally it is obvious that the size of austenite blocks decreases in
ausformed samples. This can be related to more severe nucleation of bainitic subunits, higher
volume fraction of bainitic sheaves and more decomposition of primary austenite in this set of
samples.

6
 Fig. 2. Optical micrographs of samples a) Non ausformed/2h, b) ausformed/2h, c) Non
ausformed /4h, d) Ausformed /4h, e) Non ausformed /6h, f) Ausformed /6h, g) Non ausformed
/16h and h) Ausformed /16h.

Fig. 3. Approximate alignment of bainitic sheaves with respect to the rolling direction in optical
micrographs for samples austempered for a) 6 h and b) 16 h.

The strength of austenite is the main factor controlling the size and thickness of the bainitic
subunits [20, 46]. Moreover, keeping in mind that bainitic ferrites grow through a displacive
mechanism which involves a coordinator movement of atoms [47-49], an assumption is to gain
more refined microstructure after ausforming the samples because ausforming can have a
detrimental effect increasing the dislocation density and strength of retained austenite which can
further resist the austenite/ferrite glissile interface motion. High magnification FE-SEM
micrographs for samples austempered for 6h, see Fig. 4, illustrate that it was possible to achieve
bainitic subunits of almost 642nm and 683nm thicknesses in ausformed and non-ausformed
conditions respectively. Austenite films measured to have almost the same thickness. Therefore,
results indicate that 10% of ausforming could not be that much effective to further refine the

7
microstructure and maybe higher amount of plastic deformation of austenite was mandatory to
achieve more refined microstructure.

Fig. 4. High magnification SEM micrographs of a) non-ausformed and b) ausformed samples,

austempered for 6h.

Fig.5 depicts the variations of the volume fraction of retained austenite and hardness with
austempering time. According to the figure, the volume fraction of retained austenite increases to
a maximum value at heat treatment time where bainite transformation is supposed to be
completed. This is logical assuming that higher bainitic ferrite forms by increasing the heat
treatment time. So, the volume fraction of austenite blocks decreases, higher amount of C rejects
to surrounding austenite, makes it thermally more stable and forbids its transformation to
martensite during cooling to room temperature. Consequently, replacing harder martensite by
bainite within the microstructure by increasing the austempering time decreases the materials
hardness. However, it is evident that hardness again increases in both sets of samples when
austempering for 16 h. This can be related to cementite precipitation at prolonged austempering
times further than that of needed for bainite transformation completion [50]. The decrease in C
content of austenite due to the precipitation may impoverish it sufficiently to become thermally
less stable and to transform to martensite during cooling to room temperature. This results in a
slight decrease of austenite content after 6 h even if it is not that much considerable, see Fig. 5. a.
This phenomenon will be more obvious if there are higher amount of bigger blocky austenites in
the microstructure as they are more susceptible to lose their thermal stability due to their lower C
contents comparing to that of austenite films which is the case of non ausformed samples.

8
 Fig. 5. a) Volume fraction of retained austenite and b) hardness variations at different
austempering times.

According to the figures, ausformed samples have more retained austenite at every austempering
stages. This can be rationalized based on the lower thermal stability of blocky austenites. So far,
increasing the volume fraction of the bainitic sheaves and consequently decreasing the austenite
block sizes and volume fractions by ausforming make them to be enriched enough with carbon to
resist martensitic transformation during cooling to room temperature. So it is logical to have
more retained austenite in ausformed samples because of their smaller austenite blocks and being
richer in C and thermally more stable. For instance, microstructural evaluations demonstrated
that the austenite block sizes decrease from 1200  83 nm in non-ausformed sample to 810  67
nm in ausformed sample austempered for 6h. Therefore, the higher volume fraction of retained
austenite within the microstructure of the ausformed samples makes it reasonable to attain lower
hardness values contrary to the fact that they are work hardened and contain higher dislocation
densities.

Fig. 6 depicts the impact toughness test results in both non-ausformed and ausformed test
specimens at each austempering time. It is clear that the impact energy increases by
austempering time in both cases and after a maximum it again decreases. Moreover it is clear
that the impact energy for ausformed samples is higher than that of non-ausformed specimens
after 2 and 4h austempering time. But samples austempered for 6 and 16h have lower impact
energies.

9
 Fig. 6. Impact energy variations with austempering time.

In addition, SEM fractographic analysis of both austempered samples confirms that fracture
mode is cleavage/quasi cleavage in both sets of samples an example of which is given in Fig. 7
for samples austempered for 4h.

Fig. 7. Fracture surfaces of a) non-ausformed and b) ausformed samples austempered at 4h.

The volume fraction of retained austenite present within the microstructure is a critical factor
influencing the impact toughness in nanostructured bainitic steels through its crack blunting
effect, the stress relief and the martensitic transformation ahead of the cracks [51]. So it is logical
to achieve improved impact toughness by increasing the austempering time in both ausformed
and non-ausformed samples up to austempering time of 6h. Because, in both cases, the
microstructure consists of bainitic ferrite, retained austenite and martensite at earlier stages of
transformation where later deteriorates the toughness properties because of being a brittle
constituent. However, martensite replaces by austenite and bainite by increasing the
austempering time which enhances the impact energy. However, as it has mentioned before,

10
austenite may lose its thermal stability at prolonged austempering times and may transform to
martensite during cooling to room temperature, Fig. 5. a. This again reduces the impact energy in
both ausformed and non-ausformed samples.

When comparing the impact toughness variations in ausformed and non-ausformed samples at
each identical austempering time, care must be taken that not only the volume fraction of the
retained austenite but also its morphology are determining factors [52]. TRIP effect of
moderately stable austenite can increase the impact toughness of nanostructured bainite.
However, it is well known that, austenite blocks are more susceptible to martensitic
transformation due to the lower mechanical stability [26]. Then, they cannot effectively restrict
the crack growth and increase the impact toughness. Therefore it will be beneficial to replace
austenite blocks with austenite films as much as possible. According to the results, ausforming
increases the bainitic ferrite and austenite films volume fraction, decreases the amount of
martensite and reduces the austenite block sizes and consequently ausformed samples contains
higher amount of mechanically more stable retained austenite. Therefore it seems to be logical to
gain higher impact toughness values for ausformed samples at 2h and 4h of austempering times.
However, it is in contradiction with results of impact energy measurements in samples
austempered for 6h and 16h where ausformed samples supposed to have higher values based on
this theory. This can be rationalized keeping in mind that bainitic sheaves and their morphologies
also play a significant role during the propagation and growth of cracks. Sheaves are capable of
arresting/deflecting the cracks in the packets and plate boundaries. So, bainitic sheaves with
different crystallographic orientations will improve toughness effectively by changing the crack
growth path repeatedly. However, ausforming decreases the number of the bainite variants. This
strong variant selection overcomes the beneficial effect of higher volume fraction of moderately
stable retained austenite. That is why ausformed samples renders lower impact energy values
after austempering at 6h and 16h contrary to their higher volume fraction of retained austenite,
more filmy austenites, refined austenite blocks and lower martensite. These strong variant
selections were even evident in SEM micrographs of fracture surface of ausformed samples an
example of which is illustrated in Fig. 8 for ausformed sample austempered for 6h. Elongated
dimples are evident in these micrographs with different magnifications and some are marked
with arrows.

11
 Fig. 8. Fracture surfaces of ausformed samples austempered for 6h at a) lower and b) higher
magnifications.

As it has noted before, presence of microstructural bandings within the microstructure due to the
Mn segregation can decrease the impact toughness energy. The boundaries of bainitic sheaves
and these bands act as potential sites of crack nucleation [19]. However, precise microstructural
evaluations in many different low magnification optical pictures from different sections of the
heat treated materials in this study, failed to reveal any severe banding evidences.

Conclusions

It has been demonstrated conclusively that the ausforming can influence the transformation
kinetic, microstructural characteristics and impact toughness in nanostructured bainitic steels.
Results show that bainitic transformation can be accelerated by ausforming prior to isothermal
bainitic heat treatment especially at earlier stages. Moreover, ausforming successfully increases
the volume fraction of high carbon retained austenite within the microstructure and refines the
austenite blocks. Furthermore, bainitic sheaves tend to grow in limited crystallographic variants
comparing to that of non-ausformed samples because of the inhomogeneous plastic flow of
individual austenite grains after ausforming.

Ausforming enhances the impact toughness energy absorbed in samples austempered for 2 and
4h. This can be rationalized based on the higher volume fraction of ductile austenite present
within the microstructure of ausformed samples. However, it is crucial to note that not only high
carbon retained austenite, but also bainite sheaves and their morphologies must be considered
when talking about impact toughness. Sheaves of bainite play an important role during the
propagation and growth of a crack where growing sheaves at much more different
crystallographic orientations improves toughness effectively by changing the crack growth path

12
repeatedly. So, variant selection of bainitic sheaves in ausformed samples austempered at longer
austempering times of 6 and 16 h deteriorates the impact toughness despite the higher volume
faction of ductile austenite.

Acknowledgment

Authors are grateful for Sahand University of Technology for supplying research facilities for
this work.

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