E3S Web of Conferences 355, 02008 (2022) https://doi.org/10.

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Formation of thermal oxide scale and its adhesion to

hot-rolled low carbon steels with different final strip
thicknesses
Sun Naipinij, Sasapan Sukieum, Ravinupha Namprai, and Thanasak Nilsonthi*
High Temperature Corrosion Research Centre and Department of Materials and Production Technology Engineering, Faculty of
Engineering, King Mongkut’s University of Technology North Bangkok, 1518, Pracharat 1 Road, Wongsawang, Bangsue, Bangkok,
10800, Thailand

Abstract. Currently, the steelmaking industry produces iron oxide waste scale resulting in pollution to the
environment. It was necessary to have a good understanding of the composition, characteristics and properties
of the oxide scale. This study focused on the formation of scale and its adhesion to the hot-rolled steel strip
with different thicknesses. The oxide scale formed on an as-received hot-rolled steel strip was investigated by
X-ray diffraction (XRD), scanning electron microscopy equipped with energy dispersive X-ray (SEM-EDS).
Magnetite, hematite and iron were found from the XRD results of all samples, which had the thickness strip
of 8, 10 and 12 mm. The scale was thinner for the thinner strip. The adhesion test was conducted by a tensile
testing machine adapted with an observation set. The strain initiating the first spallation and mechanical
adhesion energy was lowest for the sample with the highest thickness (12 mm). These results indicate that the
waste scale produced by hot rolled steel industry can be controlled by the final strip thickness. There was a
need to control the scale of waste in a reasonable way to protect the environment.

Keyword. Waste scale, Iron oxide, Rolling mill steel, Hot-rolled steel, Strip thickness, Adhesion

1 Introduction scale rather than forming internal oxidation. Due to

eutectoid decomposition during cooling, magnetite can be
The thermal oxide scale formed on the steel surface occasionally found in the wustite layer. The hematite
because of the process temperature in the hot rolling line, layer may also be absent in some cases.
which is around 600-1250°C. It is de-scaled both, first In the hot rolling process, a slab is rolled at high
before the slab enters the roughing mill and again before temperatures in order to obtain a strip with desired
the steel bar enters the finishing mill, using a high- thickness [14]. At high temperatures, the steel reacts with
pressure water jet. Thermal oxide scale continues to rapid oxygen in the ambient atmosphere and gives a thermal
form during steel strip coiling and storage after the second oxide scale [1-13]. The oxide formed is a waste of the
de-scaling, until the temperature decreases below 400°C. process and it should be minimised. Many factors can
The existence of this scale has a significant impact on the affect the amount of the scale formation, such as alloying
product's quality. elements in the steel like C [15], Si [16], Cu [17], Sn [18]
A slab is a raw material for making carbon steel strips or Ti and Nb [19] or the parameters set in the process
in a hot rolling line, and it can be made in one of two ways: [20-22]. The objective of this work is first to investigate
blast furnace (BF) or electric arc furnace (EAF). A if the final strip thickness relates to the amount of oxide
blast-furnace route can be used to make a slab from iron formation.
ore, coal, and limestone. For the electric arc furnace route, In addition, the amount of oxide formation can affect
steel scraps are the main raw material for making a slab, the adhesion of scale to steel. This property is important.
tramp elements in steel were present in the slab and might If the hot-rolled steel is delivered to the customer for the
affect the thermal oxide scale structure. This may have an direct application in this form, good scale adhesion is
impact on the pickling behaviour in the following pickling required. If the hot-rolled has to be successively
line. cold-rolled, the bad scale adhesion is preferred. This is
During the hot rolling process, steel is oxidised and a because the scale can be easily removed from the steel
scale of iron oxide formed on the steel surface at process surface before further cold rolling. The adhesion of oxide
temperature comprises three layers a thin outermost scale on steel substrate can be assessed in many ways,
hematite (Fe2O3), an intermediate magnetite (Fe3O4), and such as the indentation test [23], the inverted blister test
a thick inner wustite (FeO) [1-13]. For the Fe-O system, [24, 25], the bending test [26-29] or the tensile test [30-
the scale layer can vary via concentration gradients of 34]. Our group developed the tensile test [35-39] to
oxygen. An iron oxide formed always grows external evaluate the scale adhesion of low carbon steels [15, 19,

*
Corresponding author: thanasak.n@eng.kmutnb.ac.th

© The Authors, published by EDP Sciences. This is an open access article distributed under the terms of the Creative Commons Attribution License 4.0
(http://creativecommons.org/licenses/by/4.0/).
E3S Web of Conferences 355, 02008 (2022) https://doi.org/10.1051/e3sconf/202235502008
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22, 35-39] and stainless steels [40-42]. It will be used in by product specification. Considered to phase
this study. The structure and adhesion of the oxide scale transformation when exiting the hot rolling mill, the
after the hot rolling process are focused on in this study. choice of finishing and coiling temperatures have a
The effect of final strip thickness on scale formation and significant influence on achieving product property. Table
adhesion is emphasised. During the industrial production 1 shows the chemical composition of the steel. Table 2
of steel, tons of iron-rich scale are produced as waste shows the information from mechanical tensile testing.
materials [43]. The waste contains large amounts of iron
oxides, heavy metals and other different contaminants. It Table 1. Chemical composition of the as-received hot-rolled
steel strip (wt.%).
affects the environment when disposed of in landfills [44].
The environment is polluted. The scale as a process waste Sample C Si Cu Mn P S
should be kept to a minimum. 8 mm 0.138 0.006 0.010 0.441 0.017 0.009
For preventing scale formation in steel industries, 10 mm 0.156 0.007 0.009 0.454 0.016 0.002
since the scale formation during the hot rolling process at 12 mm 0.158 0.009 0.007 0.440 0.020 0.006
high temperatures. Several hot rolling conditions have
been proposed to prevent the scale problem. Control of Table 2. The tensile mechanical properties of a material.
slab heating temperature and alloying elements content Mechanical properties
are some of those proposed processes. However, these Strip Yield Tensile
conditions are not sufficient in preventing scale defects in Elongation
thickness strength strength
the commercial hot rolling process. The thick scale (mm)
(MPa) (MPa)
formed during heating for a long time in the furnace and 8 mm 444 502 18
remains even after water jet descaling. A short time 10 mm 348 441 29
holding in the furnace might control this scale. The 12 mm 385 463 27
existence of fayalite (Fe2SiO4) for high Si steel is an
additional important factor to prevent scale formation. 2.2 Characterisation
This is due to scale thickness decreasing with the
increasing silicon content. However, the strong bonding The oxide scale morphology is observed by the scanning
of fayalite on the scale-steel interface is considered to electron microscope (SEM, QUANTA 450). The
descaling process. The scale generated by the steel plant energy-dispersive X-ray spectroscopy (EDS, OXFORD
is called waste, but now this term has been replaced with INSTRUMENTS, Model X-Max) was equipped with
a by-product. Mill scale is one of the by-products SEM for elemental analysis. The oxide phase is
produced during steel processing. Mill scale is used for determined by the X-ray diffraction technique (XRD,
magnetic storage, polishing, chemical manufacturing, SmartLab) using the Cu Kα line (k = 0.15406 nm) with a
pigment manufacturing, and biomedical application. step size of 0.02 degree/step and a step time of 0.5
second/step.
2 Materials and methods
2.3 Mechanical adhesion
2.1 Materials The tensile testing machine (Instron, Model 5566) with a
load of 10 kN is used. The strain rate of 0.04 s-1 at room
The study used hot-rolled steel which is available from temperature is operated. A high-magnification lens with a
Sahaviriya Steel Industries Public Company Limited as a CCD camera has been used to observe the evolution of
strip with a thickness of 8, 10 and 12 mm. The position of scale failure. The video processing is performed at a
the hot-rolled coil at the head, middle and tail are used for resolution of 640 × 480 pixels. Image framework
examination as shown in Figure 1. The sample is cut from programming is used to acquire the image. The CCD
a strip obtained from a slab produced by the blast-furnace camera has a frame rate of 7.5 frames per second. The
route. In the hot rolling process, the finishing and coiling specimen is prepared according to the ASTM E8M
temperatures of the sample, which had a strip thickness of standard. Figure 2 shows the tensile testing machine with
8 mm are 790°C and 580°C respectively, for the strip the scale observation set and sample shape.
10 mm is 780°C and 590°C, for strip 12 mm is 760°C and
560°C.
3 Results and discussion
Figure 3 presents cross sections of the 8-mm strip at the
head, middle and tail positions. The XRD pattern for each
scale was also shown in Figure 4. It was seen that the
thickness of scale at the head position was 12.82 ± 2.57
Figure 1. Position of sample in the hot-rolled coil taken for
μm. They were 16.42 ± 2.29 μm and 10.77 ± 1.15 μm at
examination. the middle and tail positions respectively. Fe2O3, Fe3O4
and Fe were found in the XRD patterns of the scale
The hot-rolled steel is used for several products e.g. formed in these three positions. The literature [4] was
pipe and tube, automotive structural, machine structures, reported the oxidation of iron and steel in oxygen or air at
and gas cylinders. The final strip thickness is considered high temperatures. At temperatures above 700°C, iron

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oxidation follows the parabolic law, resulting in the where   is an iron-rich wustite, which subsequently
formation of three-layered hematite, magnetite, and decomposed into a eutectoid product via the following
wustite. Carbon steel oxidation was generally slower than reaction.
iron oxidation. The scale structure of carbon steel was 4  →   + (1 − 4 ) (2)
similar to those formed on iron after very short-term
oxidation.

Figure 2. Tensile machine set up with observation set (a) and

sample shape (b).

The oxidation behaviour of carbon steel at high

temperatures has been extensively studied in the previous.
Oxidation behaviour of steel and scale structure was more Figure 3. Scale structures on a strip with 8 mm of thickness at
difficult to understand than iron oxidation due to the head (a), middle (b) and tail (c) positions.
presence of various alloying and impurity elements.
However, literature [45] has proposed that the steam
partial pressure was unaffected by the rate of oxidation. During wustite decomposition, primary magnetite
The hematite layer was very thin, which affects the precipitation inside the wustite phase was readily formed
oxygen activity at the magnetite-hematite interface. From and then followed by magnetite precipitation at the
this research, hematite and magnetite layers were wustite-iron interface. Finally, eutectoid forming
observed without the wustite layer. According to the Fe- magnetite and iron. In our view, high temperature
O phase diagram as shown in Figure 5, wustite will fully promoted the development of the wustite layer which was
decompose undergoes eutectoid transformation and turns possible at temperatures higher than 570°C. At
into magnetite and iron at 570°C or below during the temperatures below 570°C, the layered magnetite and iron
cooling after hot rolling. Literature [20] suggestion was a eutectoid were continuously formed. Conversely, wustite
direct magnetite-formation mechanism. The presence of could be found at temperatures below 570°C when the
an iron substrate was not essential for the formation of the cooling rate was high enough. In addition, wustite might
magnetite layer. The mechanism of forming the magnetite undergo a eutectoid reaction to form a mixture of
layer was via the following primary reaction without the magnetite and iron when oxidation was preceded under a
involvement of the iron base. continuous cooling process. The oxide scale
microstructure formed via phase transformation of wustite
  → [( − )/(1 − 4 )]  affects the surface quality of steel products. However, this
+[(1 − 4 )/(1 − 4 )]  (1) study was focused on the effect of final strip thickness in

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the simplest way for understanding the adhesion of iron

oxide waste scale from the rolling mill steel industry.
Therefore, it was necessary to have a good understanding
of oxide scale composition. Table 3 shows the
composition of the oxide scale obtained from hot-rolled
steel. The EDS mapping spectra for the sample shows that
the main elemental components were Fe, O and C. This
indicates that the iron oxide as the main phase was
presented, and the carbon-rich originate from the hot-
rolled steel. It can be noted that the presence of Si was
found on a scale of a 10 mm strip thickness at the middle
position. It was due to Si-rich precipitates in the oxide
scale of their steel.

Figure 5. Fe-O phase diagram [46].

Figure 6 illustrates cross sections of the 10-mm strip

at the head, middle and tail positions. The XRD pattern
for each scale was also shown in Figure 7. It was seen that
the thickness of scale at the head position was 10.41 ±
3.89 μm. They were 37.44 ± 7.61 μm and 13.34 ± 3.34
μm at the middle and tail positions respectively. Fe2O3,
Fe3O4 and Fe were found in the XRD patterns of the scale
formed in these three positions.

Fig. 4. XRD patterns of the strip with 8 mm of thickness at the

head (a), middle (b) and tail (c) positions.

Table 3. Elemental quantification in percentage weight (wt.%)

obtained by EDS analysis for the scale as-received hot-rolled
steel strip.

Thick Position Fe O C Si
Head 40.26 23.74 36.00
8 mm. Middle 37.59 30.22 32.20
Tail 34.75 31.43 33.81
Head 21.64 33.64 42.45
10 mm. Middle 38.76 38.08 22.02 1.13
Tail 37.49 35.37 25.65
Head 43.26 23.31 33.44
12 mm. Middle 40.33 34.00 25.67 Figure 6. Scale structures on a strip with 10 mm of thickness at
Tail 39.91 37.26 22.82 the head (a), middle (b) and tail (c) positions.

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Figure 7. XRD patterns of the strip with 10 mm of thickness at

head (a), middle (b) and tail (c) positions.
Figure 8. Scale structures on a strip with 12 mm of thickness at
the head (a), middle (b) and tail (c) positions.
Figure 8 shows cross sections of the 12-mm strip at the
head, middle and tail positions. The XRD pattern for each
scale was also shown in Figure 9. It was seen that the
thickness of scale at the head position was 29.44 ± 2.63
μm. They were 45.13 ± 8.99 μm and 74.36 ± 6.54 μm at
the middle and tail positions respectively. Fe2O3, Fe3O4
and Fe were found in the XRD patterns of the scale
formed in these three positions.
From XRD results, the oxide scale formed at rolling
temperatures comprises hematite and magnetite with iron
as shown in all samples. Qualitative phase analysis
provides oxide scale information gleaned from an X-ray
diffraction pattern. Each phase of a crystalline oxide will
produce a unique diffraction pattern. The diffracted peak
positions and intensities from a particular oxide phase
serve as a fingerprint that can be compared to a database
of reference patterns to identify a phase. A pattern plot of
diffracted X-ray intensity with Bragg angle. The peak
positions of the hematite phase shown at 24.17°, 33.19°,
35.66°, 40.90°, 49.51°, 54.13°, 62.49°, and 64.05° were
indexed to (012), (104), (110), (113), (024), (116), (214),
and (300) respectively. While the peak positions of the
magnetite phase shown at 30.07°, 35.42°, 43.05°, 56.93°,
and 62.51° were indexed to (220), (311), (400), (511), and
(440) respectively. The peak positions of the iron phase
shown at 44.68°, 65.03°, and 82.34° were indexed to
(110), (200), and (211) respectively. It can be noted that
the peak positions and relative intensities of the sharp
peaks in XRD patterns indicate the hematite, magnetite
and iron were well crystallised. Figure 9. XRD patterns of the strip with 12 mm of thickness at
head (a) position middle (b) and tail (c) positions.

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A comparison of the oxide scale thickness as a lower than that scale thickness was observed on as-
function of final strip thickness for specimens at the received hot-rolled steel with a final strip thickness of 8-
position of the head, middle and tail was shown in Figure 12 mm. This was due to the difference between the
10. The thickness was measured using cross-sectional thickness of the sample, oxidation temperature and
metallographic images. It was found that the scale oxidation time.
thickness of the studied 12-mm thick strip was The oxide adhesion to a steel substrate will be
significantly increased at all positions. It was well known discussed formally in terms of oxide-steel separation. The
that the thickness of oxide scale was linear with the weight adhesion of scale on steel was previously considered [49].
gain of the scale due to the absorption of oxygen. With the Many failures occurred in the oxide near the interface,
increase in exposure time, the internal and external involving oxide growth stresses, oxide and steel plasticity,
thickness of the oxide scale gradually thickens. If the strip and thermal cycle effects caused by differential thermal
thickness is high, provide more time for cooling after the contraction. Cracks normal to the interface, cracks
hot rolling process. Scale continued to grow as a result. It parallel to the interface or spalling were all examples of
was also seen that the thickness at the tail position on a local failures. Attention was focused here on the scale
strip of 12 mm was higher than that head and middle spallation and adhesion. Figure 11 shows strain initiating
positions. This might be due to the accumulation of heat the first spallation of the strip with 8, 10 and 12 mm of
at the strip tail during the hot rolling process, thickness at the head, middle and tail positions. It was
corresponding to using a longer cooling time. The results seen that the strain resulting induced the first spallation of
indicate a drop in scale thickness when the final strip a strip with a thickness of 12 mm was lower at all
thickness was decreased. This can be attributed to the positions. This indicates that during the hot rolling
higher cooling rate of the thinner strip. While the scale process oxide scale was easier to flake off. In terms of
thickness at the middle position on strips of 8mm and mechanical adhesion energy, it was determined using
10mm seems to be higher than the head and tail positions. information from the literature [26, 50-54]. The values
Literature [47], this study was to improve the longitudinal reveal that the strip with a thickness of 12 mm has lower
performance uniformity of hot-rolled coils. The results mechanical adhesion energy at all positions as shown in
show that the average cooling rate of the head and tail Figure 12.
parts were higher than that of the middle part during coil
cooling. This might cause lower scale thickness on strips
of 8-mm and 10-mm at head and tail positions. However,
accumulation of heat at the strip tail was going to have an
effect on the strip of 12 mm. It can be observed that the
global scale thickness of the strip of 12 mm seems to be
higher.

Figure 11. Strain initiating the first spallation of the strip with
8, 10 and 12 mm of thickness at the head (H), middle (M) and
tail (T) positions.

Figure 10. Oxide scale thickness of strip with 8, 10 and 12 mm

of thickness at the head (H), middle (M) and tail (T) positions.

Comparison literature [48], this research shows the

thicknesses of oxides formed on AISI 1045 were 2.92 μm
and 6.22 μm for oxidation of 168 and 720 hours
respectively. Oxidation of steel was performed in the
heated air inside the furnace at 673 K (400°C). After the
oxidation process was completed, the sample was kept in
a desiccator for cooling down to room temperature. Note
that before oxidation the steel was cut into 20 mm in Figure 12. Mechanical adhesion energy of strip with 8, 10 and
diameter with a thickness of 2 mm. The results show that 12 mm of thickness at the head (H), middle (M) and tail (T)
the scale thickness was found in the range of 3-6 μm, this positions.

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