Journal of Chemical

Journal Technology
of Chemical and Metallurgy,
Technology 55, 1,55,
and Metallurgy, 2020, 198-209
1, 2020

MICROSTRUCTURAL IMAGE ANALYSES OF MILD CARBON STEEL SUBJECTED

TO A RAPID CYCLIC HEAT TREATMENT

Orhadahwe Thomas Aghogho1, Adeleke Adekunle Akanni2, Aweda Jacob Olayiwola1,

Ikubanni Peter Pelumi3, Odusote, Jamiu Kolawole2

1
Mechanical Engineering Department, University of Ilorin, Ilorin, Nigeria Received 25 February 2019
2
Materials and Metallurgical Engineering Department, Accepted 31 July 2019
University of Ilorin, Ilorin, Nigeria
3
Mechanical Engineering Department, Landmark University, Omu Aran, Nigeria
E-mail: [email protected]

ABSTRACT

The study is focused on using an image analysis to explain the effects of several cycles of rapid heat treatment on
the microstructure of 0.213 wt. % carbon steel. The samples examined are subjected to a diffusional heat treatment
followed by several cycles of a rapid heat treatment. The process of the diffusional heat treatment involves heating
the samples from an ambient temperature to 850oC in an electric muffle furnace for 56 min and then quenching in
running water. In order to improve further the mechanical properties of the heat treated samples, they are subjected to
several cycles of rapid heating. Each cycle comprises preheating the furnace to 900oC prior to the samples charging.
The treated samples are subjected to a microstructural examination using optical microscopy followed by an image
analysis using Image J software. The mechanical properties of the heat treated samples are characterized through
ultimate tensile, hardness and impact tests. The results reveal that the grain size decreases from 1.07 μm in the con-
trol sample to 0.79 μm in the three-cycle sample and increases to 0.86 μm in the four-cycle one. It is also observed
that the two-cycle sample shows the highest ductility (15356.3 N/mm2) and the lowest ultimate strength (833.375
N/mm2). This implies that the two-cycle rapid heat treatment is required for grain refinement in mild carbon steel.
Keywords: rapid heating, microstructure, image analysis, martensite, quenching.

INTRODUCTION strengthens the material. The grain refinement can be

achieved by rapid heating [7]. Grange [8] advances the
The specific mechanical properties of the metal possibility of austenite grains refinement by shortening
products are basic requirements for their application the austenite cycle. This can be achieved by subjecting
[1]. These properties can be obtained along different the steel to a rapid heat treatment which involves heating
strengthening mechanisms which act together during at a fast rate to its austenitic temperature and immedi-
the deformation process. The heat treatment [2] is one ate quenching without soaking. It is argued whether the
of these mechanisms because it affects [3, 4] the prod- steel soaking at this temperature is necessary. It is worth
ucts strength and toughness. The properties considered noting that the process of a rapid austenitizing treatment
improve with the grain size refining but the mechanism saves time, costs and minimizes the steel oxidation and
of the process is not entirely clear for martensitic steels decarburization. The minimization of the austenite grain
[5]. According to Muszka et al. [1] the procedure to growth leads to the formation of fine grains in the heat
strengthen a metal depends on its chemical composition, treated product.
its deformation history and the resulting microstructure. Dabkowski and Porter [9] suggest that the rapid heat
Tejas [6] assumes that the grain refinement provides treatment spanning between 5 min and 30 min has to
a different orientation of the grains preventing thus be immediately followed by quenching. According to
dislocations, crack initiations and failures. This in turn Twiggs et al. [10] a heating rate above 20oC/min should
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 Orhadahwe Thomas Aghogho, Adeleke Adekunle Akanni,
Aweda Jacob Olayiwola, Ikubanni Peter Pelumi, Odusote, Jamiu Kolawole

be considered a fast one. In fact the rapid heat treatment In addition, the study uses an image analysis to explain
involves the use of fast heating rates. The process gener- the microstructural behavior of the heat treated steel. It
ates a surface of properties which are distinctly different is a process of acquiring quantitative information on the
from those of the initial microstructure obtained through microstructural parameters of a material including size, so-
a conventional or a diffusional heat treatment [11]. The lidity, porosity and circularity. There are several software
literature data shows that the temperature and the time programs designed to carry out this analysis. They refer
of the heat treatment process affect the mechanical to Amira, Consol multiphysics and Image J [19]. Despite
properties. It is so because the increase of the heating the increasing application of the image analysis, there are
rate leads to smaller, equixed grains of increased hard- only a few references [19, 20]. Image J software is used
ness, yield and fatigue strength [12]. Grange [8] states in the present investigation and aimed at elucidating the
that one or two cycles of a rapid heat treatment would effect of the rapid cyclic heat treatment on mild steel
produce ultra-fine mild steel grains of increased strength microstructure.
and toughness. However, there is no verification of this
claim. There are several studies on the application of EXPERIMENTAL
a rapid heat treatment of other steel grades [9 - 13]. Sample preparation
There are also several investigations on thermal cycling The elemental composition of the AISI 1021 steel
[14 - 17] but none of them focuses on the effect of the sample was obtained using optical electron spectrometry.
rapid cyclic heat treatment of mild steel. Lv et al. [18] The data obtained is presented in Table 1. It was found
accept that the traditional route of a cyclic heat treat- that the steel sample contained 0.213 wt. % of carbon
ment involves preheating and repeated quenching and which qualified it as mild steel [21, 22].
tempering which is time consuming. The material used was cut and machined to the re-
The method used in this study applies several cycles quired tests dimensions with the aid of a lathe machine.
of rapid heating and quenching which decreases the heat The samples were then labeled for the various cycles of
treatment demands in respect to time, energy and cost. the heat treatment as shown in Table 2.
This study verifies also the claim of Grange [8] that one
or two cycles of a rapid heat treatment would provide Initial diffusional heat treatment
strength and toughness in mild steel. The study is aimed The diffusional (conventional) heat treatment pro-
at the determination of the exact number of the cycles cedure for producing martensitic steels involves slow
required to result in toughness and ductility increase in heating to austenite and rapid cooling of austenized
the mild steel subjected to a quenching heat treatment. specimen in a quenching medium [23]. All samples

Table 1. Chemical composition (wt. %) of the steel sample.

C Si S P Mn Ni Al W
0.213 0.252 0.030 0.028 0.779 0.131 0.292 <0.0001
Cr Mo V Cu Nb B Ti Fe
0.138 0.020 0.030 0.336 0.014 0.001 0.009 97.700

Table 2. Sample identification tag based on various cycle of treatment.

Sample Control (A) One cycle Two cycle Three cycles Four cycles (E)
(B) (C) (D)

Heat Diffusional Diffusional Diffusional Diffusional Diffusional

treatment heat and one and two and three heat treatment
treatment cycle of cycles of cycles of and four cycles
only rapid heat rapid heat rapid heat of rapid heat
treatment treatment treatment treatment

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were subjected to a diffusional heat treatment which Metallographic examination/Image analysis

involved slow heating from a room temperature to the Five sets of specimen were prepared for metallo-
austenite one (852 ℃) and soaking for 10 min [24, 25]. graphic examination. The procedure involved grinding
The austenized steel samples were then rapidly cooled the treated steel samples to produce a flat and smooth
using tap water. The heating and the cooling rates were surface. Silicon carbide paper of different grades (220,
determined electronically with a thermocouple con- 320, 400 and 600) placed on a grinding machine was
nected to the data logger. used. Subsequently the samples were polished using a
selvet cloth swamped with a solution of 1-micron and
Cyclic rapid heat treatment 0.5-micron silicon carbide to produce a mirror like sur-
The electric muffle furnace was preheated to 900℃ face. The samples were etched to reveal the boundaries
to increase the heating rate of the charged samples. It of the polished surface using 2% Nital (2 % nitric acid
was found that the samples were heated from an ambient and 98 % alcohol). Then they were washed, dried and
temperature to 852oC within 10 min. Then the samples viewed with an accuscope optical microscope at 400x
were quenched in tap water. This procedure constituted magnification. The image analysis was carried out using
a cycle. Experiments with samples exposed to one, two, Image J software following the flowchart in Fig. 1 [19,
three and four cycles were carried out aiming to verify 26]. The grain sizes were determined by the planimetric
the claim of Grange [8]. method in accordance with ASTM E112-13 [27].

Sample preparation

Image acquisition

Image filtering
Gray tone Illumination
RGB Image Conversion Correction

Image segmentation
Thresholding Topological
Segmentation
Gray-level thresholding
Watershed binarization
Skeleton cleaning

Invert image

Pore fraction Arithmetical sum

Skeleton cleaning

Invert image

Feature Math. Morphology

(Erosion )

Properties measurement
- Grain size
Measurement
Statistical analysis
- Pore fraction
Measurement

Fig. 1. Flowchart of Image J process [13].

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 Orhadahwe Thomas Aghogho, Adeleke Adekunle Akanni,
Aweda Jacob Olayiwola, Ikubanni Peter Pelumi, Odusote, Jamiu Kolawole

Mechanical properties is equal to 54.98℃/s. This implies that the cooling is

The Brinell hardness was determined using Brinell rapid leading [31, 32] to a martensic microstructure at
hardness tester in accordance with ASTM E10-15 [28] a room temperature. Fig. 4 shows the schematic repre-
standard. The Impact test was carried out using Charpy sentation of a cyclic rapid heating process. The heating
V-notch impact tester according to ASTM A370-10 [29] rate obtained amounts to 84 ℃/min. This implies that
standard while the ultimate tensile test was conducted on the heating process is fast [10]. The possibilities of grain
an universal testing machine following ASTM E8 [30]. size refinement via this process are high [33].
All mechanical properties were evaluated electronically.
Three samples were used for each cycle and the corre- Image analysis
sponding average values were obtained. Fig. 5 shows the microstructural images of the
samples. The samples subjected to rapid cooling from
RESULTS AND DISCUSSION its austenitic temperature to a room temperature attain
Heating and cooling rates a martensite microstructure [25, 31 - 32]. This is so
The diffusional heat treatment curve is presented because the fast cooling rate does not provide carbide
in Fig. 2. The value of the heating rate of the initial dif- particles even diffusion into the iron matrix. This results
fusional heat treatment is equal to 15.90℃/min. Based in jamming of the carbon lattice of the ferrite atomic
on the assertion of Twiggs et al. [10], a heating rate less arrangement. Martensite is therefore an aggregate of
than 20℃/min corresponds to slow heating. Hence, the ferrite and cementite [34].
heating used in this study is categorized as a slow one. The martensite grains are very coarse. This deter-
Therefore, it is expected that complete austenitization mines the mottled contrast of Fig. 5(a). The black areas
of the steel [24, 25] will be achieved. Fig. 3 shows the of the microstructures refer to the carbide particles [35].
cooling curve. The cooling rate at the quenching start They are greater in number in the control sample. The
black areas decrease in the course of the treatment ap-
plied giving room to a finer microstructure of improved
mechanical properties referred by Grange [8] to a fine
martensite. Figs. 5(b), 5(c), 5(d) and 5(e) illustrate
one cycle, two cycles, three cycles and four cycles of a
rapid heat treatment, respectively. The treatment applied
provides direct transformation of some of the martensite
particles to austenite without passing through the inter-
mediate phases (this is called displacive transformation).
The carbon particles however are given more room to
diffuse out and realign. This leads to a more evenly
Fig. 2. Diffusional heating curve.

Fig. 4. Schematic representation of cyclic rapid heating

Fig. 3. Cooling curve for diffusional heat treatment. process.

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Fig. 5. Microstructure of samples at 400x magnification (a) control (b) one cycle (c) two cycles (d)
three cycles (e) four cycles.

distributed microstructure on quenching. The process re- gets refined on quenching and the mottled contrast of
sults in finer grains formation due to their nucleation and Fig. 5(a) gradually becomes brighter.
the corresponding boundaries formation [36]. According Fig. 6 shows the threshold (black and white) view of
to Bhadeshia [33], the nucleation rate is accelerated by the microstructures. The black areas refer to the carbide
refining the austenite grain size as the density of nuclea- particles. They are most visible as clusters in case of
tion sites increases inversely with the austenite grain the control sample (Fig. 6(a)) and the one-cycle sample
size. The rapid heating prevents the growth of austenite (Fig. 6(b)), while the two-cycle sample (Fig. 6(c)) shows
grain size. Furthermore, the martensite microstructure fewer clusters of carbide particles in the iron matrix.
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Aweda Jacob Olayiwola, Ikubanni Peter Pelumi, Odusote, Jamiu Kolawole

Fig. 6. Threshold view of microstructures (a) control (b) one cycle (c) two cycles (d) three cycles (e) four cycles.

There is a progressive increase of these black spots in the μm2 in the control sample to 27.89 μm2 in the two-cycle
three- (Fig. 6(d)) and four-cycle samples (Fig. 6(e)). This sample. It increases to 29.26 μm2 in the four-cycle
shows that after two cycles of rapid heating, a jamming sample. It is evident that the two-cycle sample has the
of carbide particles starts to form again in the selected smallest average area. It is worth adding that two cycles
mild steel sample. This trend is also evident in Fig. 7 of rapid heating result in a decrease of the grain area of
which displays the map drawing of the microstructure. It the selected steel sample, while the further cycles lead
indicates that the two-cycle sample (Fig. 7c) has a more to a corresponding increase of the grain area.
even mixture of carbide and ferrite particles. Fig. 9 displays the surface plot (3D view) of the
Fig. 8 shows the area count of the microstructures. microstructure. It shows that green portions revealing
The effect of several cycles of rapid heating is evident (Fig. 9(a)) a cluster of carbide particles which do not
as the mean area of the samples decreases from 28.45 align properly in the iron matrix dominate the control

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Fig. 7. Map (drawing) of microstructure (a) control (b) one cycle (c) two cycles (d) three cycles (e) four cycles.

sample. These green portions are gradually replaced by presented in Table 3. The results show that the total
pink and blue one in the one-cycle sample plot (Fig. 9(b)) area decreases from the control (1153849 μ𝑚2) to the
indicating the gradual realignment of the particles in the two-cycle sample (249739 μ𝑚2) and increases for the
martensite matrix. After two cycles of a rapid treatment, four-cycle sample (859164 μ𝑚2). Similarly, the circular-
most of the green portions observed in Fig. 9(a) are ity of the samples, which is a measure of how close an
replaced by a pink portion as shown in Fig. 9(c). This object is to a true circle [19], also decreases from the
implies that there is an even distribution of the carbide control sample (0.801 μm) to the two-cycle one (0.769
particles in the iron matrix structure. Subsequent cycles μm) and then increases to the four cycles sample (0.799
of a rapid heating result in a reappearance of the green μm). The maximum ferret diameter often referred to
portion as shown in Figs. 9(d) and 9(e). as ferret diameter, represents the longest dimension
The values of the image analyses parameters are of the particle independent of its angular rotation [37,

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Aweda Jacob Olayiwola, Ikubanni Peter Pelumi, Odusote, Jamiu Kolawole

Table 3. Image analyses parameters of samples.

Sample count Total Area Average Size Perimeter IntDen Circularity
Control 2499 1153849 461.72 57.31 11739.70 0.80
1-cycle 2877 1152582 400.62 41.69 50569.19 0.80
2-cycles 970 249739 257.46 54.29 65653.04 0.77
3-cycles 2633 663536 252.01 52.73 64261.94 0.79
4-cycles 2980 859164 288.31 52.49 73519.07 0.80
Sample Solidity Feret Feret X Feret Y Feret Angle Min Feret
Control 0.856 12.86 890.21 719.91 108.63 7.58
1-cycle 0.853 11.87 864.02 765.07 109.17 6.83
2-cycles 0.843 15.37 481.31 439.31 114.44 8.47
3-cycles 0.854 14.52 973.41 760.49 108.03 8.42
4-cycles 0.856 13.09 900.01 742.14 107.54 7.26

*The unit of Feret, Feret X, Feret Y, Min Feret, perimeter, IntDen and average size is μm; total area is μm2 while
the unit of Feret angle is degree.

38). The ferret diameter varies from 12.957 μm in the samples. It is evident that the two-cycle sample has
control sample to 15.374 μm in the two-cycle sample. It the lowest Young modulus value (15.36 GN/m2). This
is also observed that ferret X, ferret Y, ferret angle and indicates that it is the most ductile sample among the
minimum ferret vary in a similar pattern. tested one because ductile materials usually exhibit low
Fig. 10 displays the pictorial view of the samples Young modulus values according to Callister [39]. The
grain size. It is evident that there is a decrease of the ultimate tensile strength decreases from 1.25 GN/m2 in
grain size from 1.07 μm in the control sample to 0.79 the control sample to 0.83 GN/m2 in the two-cycle one
μm in the three-cycle one. However, there is an increase and increases to 27.77 GN/m2 in the four-cycle sample.
of the grain size of the four-cycle sample which shows This implies that the ultimate strength of the material
that the further cycles of the rapid heat treatment will decreases with the ductility increase. The results also
not lead to production of smaller grains. reveal that there is an increase of the Brinell hardness
number – it changes from 271 in case of the control sam-
Mechanical properties of the sample ple to 562.7 for the four-cycle one. Similarly, the impact
Table 4 displays the mechanical properties of the energy increases from 46.8 J for the control sample to

Table 4. Mechanical properties of samples.

Samples YM (GN/m2) UTS (GN/m2) BHN IE (Joules) EA (N.m)
Control 22.65 1.25 271.00 46.80 230.98
1-Cycle 16.40 1.03 284.00 51.20 296.17
2-Cycles 15.36 0.83 323.00 55.40 235.15
3-Cycles 20.61 1.11 377.70 61.50 265.99
4-Cycles 27.77 1.32 562.70 64.60 253.65

*YM-Young Modulus, UTS - Ultimate Tensile Strength, BHN - Brinell hardness number, IE-Impact
Energy, EA- Energy Absorbed.

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(a) (b)

(c) (d)

(e)

Fig. 8. Area of microstructures (a) control (b) one cycle (c) two cycles (d) three cycles (e) four cycles.

64.6 J for the four-cycle one. This indicates that the rapid This implies that the one-cycle sample has the greatest
cyclic heating increases mild steel hardness and impact toughness because materials of good toughness absorb
energy. The results also show that the one-cycle sample more energy to fail. It has also a good combination of
absorbs the greatest energy (296.17 J) prior to a failure. ductility and ultimate strength [40].

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Aweda Jacob Olayiwola, Ikubanni Peter Pelumi, Odusote, Jamiu Kolawole

Fig. 9. Surface plot of microstructures (a) control (b) one cycle (c) two cycles (d) three cycles (e) four cycles.

Fig. 10. Grain size of samples.

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CONCLUSIONS and toughness of low alloy martensitic steel, J. Mat.

The present study is carried out to analyze the effect Sci. Techn., 23, 5, 2006, 659-664.
of the cyclic rapid heat treatment on mild carbon steel 6. R. Tejas, What is grain refinement? Available at
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Alo, F.I. of the Department of Metallurgical Engineer- due to laser surface treatment of a high nitrogen
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