International Journal of Structural Integrity

Study on the evolution mechanism of oxidation and copper diffusion and

precipitation phenomena and their effect on the surface quality of steel plates
Spyros Papaefthymiou Constantinos Goulas Vasiliki Panteleakou
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Spyros Papaefthymiou Constantinos Goulas Vasiliki Panteleakou , (2015),"Study on the evolution
mechanism of oxidation and copper diffusion and precipitation phenomena and their effect on the
surface quality of steel plates", International Journal of Structural Integrity, Vol. 6 Iss 2 pp. 214 - 224
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IJSI
6,2
Study on the evolution
mechanism of oxidation
and copper diffusion and
214 precipitation phenomena
Received 13 August 2013
Revised 12 November 2013
Accepted 22 January 2014
and their effect on the
surface quality of
steel plates
Downloaded by La Trobe University At 07:39 22 May 2016 (PT)

Spyros Papaefthymiou, Constantinos Goulas and

Vasiliki Panteleakou
R&D Projects & Steel Physical Metallurgy, Hellenic,
Research Center for Metals – ELKEME S.A., Athens, Greece

Abstract
Purpose – Identification of the critical process conditions that enhance Cu diffusion in
ferrite grain boundaries and promote precipitation of Cu-rich particles in the proximity of steel
semi-finished products surface is crucial for every steel maker as it leads to the creation of hot
shortness cracks in final products deteriorating surface condition. The purpose of this paper is to
reveal the possible effect of Cu segregation in the metal/oxide interface, its role in surface crack
initiation and, finally, to propose actions to prevent from hot shortness issues throughout the
production chain of steel products.
Design/methodology/approach – The here presented study was based on S355 steel plate
production starting from re-melting of scrap in an EAF, followed by metallurgical treatment in a Ladle
Furnace, continuous casting, re-heating (RH) and thermo-mechanical rolling in a reversing mill. For the
purposes of this study, more than ten heats, 100 t of steel each, were analyzed. Here presented are
depicted steels in the high and low end of the permitted Cu-wt-% spectrum, 0.4 wt-% Cu (0.15 wt-% C,
1.1 wt-% Mn, VTi micro-alloyed steel) and 0.25 wt-% Cu (0.09 wt-% C, 1.2 wt-% Mn, NbTi micro
alloyed steel), respectively.
Findings – Although Cu levels of 0.25-0.40 wt-% are well below the Cu solubility in austenite
and ferrite (8 percent wt-% and 3 wt-% Cu, respectively) and within specifications, precipitation
of Cu-rich particles is observed in industrial semi-finished and/or final products. Cu-rich precipitates
and Cu segregation along grain boundaries near the steel surface lead to hot shortness cracks in
industrial products.
Research limitations/implications – Hot shortness surface defects related to Cu presence
in steel having significantly lower Cu amounts than its maximum solubility in austenite and
ferrite does not make sense in first place. Correctly, Cu is expected to remain in solid solution.
Identification of Cu-rich particles is explained on the basis of the development of double diffusion
actions: interstitial diffusion of carbon (decarburization) and substitution diffusion of copper.
Root cause analysis and reliable countermeasures will save financial and material resources
during steel production.
International Journal of Structural
Integrity
Vol. 6 No. 2, 2015
pp. 214-224 The authors would like to express their gratitude to the SIDENOR management for their co-
© Emerald Group Publishing Limited
1757-9864
operation in carrying out industrial trials, measurements and quality control with efficiency and
DOI 10.1108/IJSI-08-2013-0018 enthusiasm.
 Originality/value – Automobile scrap re-melting results in noticeable Cu amounts in EAF produced Surface
steel. Presence of Cu-rich particles in grain boundaries near the surface of intermediate or final
products deteriorates surface quality through relevant surface defects. Identification of Cu-rich
quality of steel
particles is explained on the basis of the development of double diffusion actions: interstitial diffusion plates
of carbon and substitution diffusion of copper. Pre condition for metallic Cu precipitation in ferrite is
the Cu amount to be above 3 wt-%, which is ten times higher than the usual permitted Cu amount in
such steel grades. This pre-condition is met through austenite oxidation during RH.
Keywords Cu precipitation, Diffusion, Decarburization, Hot shortness 215
Paper type Technical paper

1. Introduction – definition of the problem

Automobile scrap re-melting results in noticeable copper (Cu) amounts in Electric Arc
Furnace (EAF) produced steel. Presence of Cu-rich particles in grain boundaries near
the surface of intermediate or final products (slabs/billets and long products/plates,
respectively,) deteriorates surface quality through relevant defects. Surface defects
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appear usually as hot tears in the surface of “as-cast” material and lead to flakes and
tears in the plates after hot rolling.

2. Scope of the study

Identification of the critical process conditions that enhance Cu diffusion in ferrite grain
boundaries and promote precipitation of Cu-rich-particles in the proximity of steel semi-
finished products surface is crucial for every steel maker as it leads to the creation of
hot shortness cracks in final products deteriorating surface condition.
Scope of this work was to reveal the possible effect of Cu segregation in the metal/
oxide interface, its role in surface crack initiation and, finally, to propose actions to
prevent from hot shortness issues throughout the production chain of steel products.
For this reason real industrial data from steel plate production and findings from
industrial trials were analyzed and discussed.

3. State of the art

The continuously increasing scrap usage might be a sustainable and energy
efficient solution, but on the other hand, serious issues are raised from tramp residual
elements that compromise the final product production (Shibata and Mishima, 1997).
Such an element is Cu, which can cause liquid metal embrittlement. Liquid Cu
penetrates the grain boundaries and loosens the connection between grains.
The deformation applied during hot rolling is pronouncing the crack formation and
propagation in the bulk material (Seo et al., 1997b; Fredriksson et al., 2001). The grain
size affects the depth of cracks caused by Cu penetration (Takemura et al., 2011).
Surface hot shortness is suppressed by the refinement of grain size in very low-carbon-
ferritic IF steels.
So far hot shortness issues caused by Cu segregation at the scale/steel interface were
treated as a standalone diffusion phenomenon. In the present study, decarburization,
oxidation and Cu precipitation are examined as a system, as these mechanisms are
found to interact with each other and jointly affect surface hot shortness. This holistic
approach contributes to the novelty of our work.
Decarburization is a diffusion-related surface degradation phenomenon, observed in
steels heated at elevated temperatures when oxidizing conditions are present. Carbon
atoms diffuse through the iron lattice with the mechanism of interstitial diffusion and
react with the oxygen of the atmosphere. This reduces the carbon content of the surface
 IJSI of the steel. As the mechanical properties of steel depend to a large extent on the carbon
6,2 content, decarburization often becomes a serious problem. Decarburization has been
studied as a standalone oxidation phenomenon extensively in the past (Birks et al.,
2006), aiming mainly to detect (Perevertov et al., 2011) and predict the decarburization
depth (Nomura et al., 2000; Choi and Van der, 2012) or the impact it has on the
mechanical properties (Prawoto et al., 2008). In this study, decarburization is examined as
216 a triggering phenomenon that enables Cu-rich particle precipitation.
Cu is placed into the iron lattice as a substitution atom, whereas carbon is an interstitial
and much smaller atom (atomic radii: carbon has 70 pm and Cu 135 pm – iron for
comparison has 126 pm). Diffusion of substitution atoms is generally much slower
than this of interstitial atoms, as also dictated by the relevant diffusion coefficients
(diffusion coefficients of C and Cu at 1,300oC: in γ-iron C diffusion is approximately
10−10 m2/s, whereas in α-iron is 10−9 m2/s. Cu diffusion is 10−12 m2/s).

4. Industrial trials
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The here presented study was based on S355 steel plate production starting
from re-melting of scrap in an EAF, followed by metallurgical treatment in
a Ladle Furnace, continuous casting, re-heating (RH) and thermo-mechanical rolling
(TMR) in a reversing mill.
For the purposes of this study, more than ten heats, 100 t of steel each,
were analyzed. Here presented are depicted steels in the high and low end
of the permitted Cu-wt-% spectrum, 0.4 wt-% Cu (0.15 wt-% C, 1.1 wt-% Mn, VTi
micro-alloyed steel) and 0.25 wt-% Cu (0.09 wt-% C, 1.2 wt-% Mn, NbTi micro-alloyed
steel), respectively.

5. Experimental
Microstructure characterization of slab- and final plate- samples was performed using
Light optical metallography (LOM) with grain structure determination by means of
image analysis. For the analysis a NIKON SMZ 1,500 stereoscope (up to 100x) and a
NIKON epiphot 300 inverted metallographic microscope (up to 1,000x) were used. The
samples were etched with Nital 2 percent solution. Additionally, scanning electron
microscopy (SEM) with EDS was also used. Cross sections in the casting direction of
the slabs and along the rolling direction of the plates were examined to reveal hot
cracks and to identify root causes.
Selected samples from intermediate and final industrial products (slabs and plates
from S355 plate production) showing various surface defects were examined. Diffusion
and oxidation considerations are discussed and correlated to industrial findings.

6. Results
Although Cu levels of 0.25-0,40 wt-% are well below the Cu solubility in austenite and
ferrite (8 percent wt-% and 3 wt-% Cu, respectively) and within specifications,
precipitation of Cu-rich particles is observed in industrial semi-finished and/or final
products. Cu-rich precipitates and Cu segregation along grain boundaries near the steel
surface lead to hot shortness cracks in industrial products.
Figures 1-5 present LOM photos from analyzed S355 slabs/plates showing:
• surface cracks;
• details of the metal/scale interface;
• the decarburization depth;
 Surface
Cu segregation along the ferrite grain boundaries quality of steel
in the plate’s surface
plates

217
Decarburization zone hot cracks

Figure 1.
Hot cracks in the
upper surface of the
slab’s sample within
the decarburized
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zone; Nital
250µm 2 percent etched

Cu particles Iron oxide layer

(Fe-Si)Ox

Figure 2.
Detail of Figure 1
showing Cu-rich
particles in the
metal/scale interface
and (Fe-Si)Ox;
25 µm as-polished

• the oxidation of the ferritic surface layer;

• Cu presence (both segregation and Cu-rich particle precipitation) along grain
boundaries; and
• hot shortness cracks.
Figure 6 presents LOM and SEM photos of the microstructure of a plate’s surface. EDS
analysis proved Cu-rich phases. Cu-rich particles were also identified in the metal/scale
interface and within ferrite grains heavily oxidized near the scale or entrapped within.

7. Discussion
EAF steel making is accompanied by increased steel scrap utilization. Automobile
recycling brings increased Cu amounts that cannot be removed from the melt. Usage of
 IJSI
Cu precipitates
6,2

218

Figure 3.
Cu-rich particles
along the grain
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boundaries; (Fe-Si)Ox Cu segregation along the

visible; as-polished ferrite grain boundaries 25µm

Cu precipitates at
metal /oxide interface

Cu along grain boundaries

Hot shortness crack
Figure 4.
Cu-rich particles
along the grain
boundaries; hot
shortness crack;
Nital 2 percent etched 25 µm

nickel is considered by some researchers (Imai et al., 1997; Garza and Van Tyne, 2005;
Seo et al., 1997a) as a possible metallurgical solution for Cu removal, but is a rather
theoretical tool as it is too expensive to be considered. Even the dilutions of the steel
melt with pig iron or direct reduced iron (DRI) in EAF steelmaking, which is standard
practice by many leading steel makers, is a costly choice.
Hot shortness surface defects related to Cu presence in steel having
significantly lower Cu amounts than its maximum solubility in austenite and
ferrite does not make sense in first place. Correctly, Cu is expected to remain in solid
solution.
Identification of Cu-rich particles is explained on the basis of the development of
double diffusion actions: interstitial diffusion of carbon (decarburization) and
substitution diffusion of Cu. Precondition for metallic Cu precipitation in ferrite is
 Downloaded by La Trobe University At 07:39 22 May 2016 (PT)

Cu Cu
particles at segregation at
ferrite ferrite grain
/scale boundaries
Cu particle
interface
entrapped in the
scale

(a) 25 µ m (b) 25 µ m (c) 20 µ m

Cu particles

Isolated Ferrite inside

Cu diffusion in the
the scale
grain boundaries
(d) 20 µ m (e) 20 µ m
RD

Notes: (a)-(b) as-polished; (c)-(e) etched plate’s surface

Plate microstructure
Surface

plates

Figure 5.
219
quality of steel
 IJSI Cu rich particles
Cu

6,2
Cu segragation
along the ferrite
grain boundaries
(b)
220 (a) 50 µm Acc.V Spot Magn Det WD 10 µm
20.0 kV 3.0 2000x BSE 5.2 Metallography&Electron Optics Dept

Cu in grain boundaries
Fe

C Sn
Mg Si

(d) 1.00 2.00 3.00 4.00

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(c) 25 µm
Acc.V Spot Magn
20.0 kV 3.0 500x
Det WD 50 µm
BSE 5.2 Metallography&Electron Optics Dept

Cu precipitates in
the Ferrite

Figure 6.
LOM and SEM (e)
photos of the
Acc.V Spot Magn Det WD 10 µm
microstructure of
20.0 kV 3.0 2500x BSE 5.1 Metallography&Electron Optics Dept
a plate’s surface;
Cu-rich particles Notes: (a)-(c) LOM photos; (b)-(d) SEM photos of the same spot; (e): higher magnification
and (Fe-Si)Oxa
SEM photo showing Cu precipitates in ferrite

the Cu amount to be above 3 wt-%, which is ten times higher than the usual permitted
Cu amount in such steel grades. This pre-condition is met through austenite oxidation
during RH in presence of oxidative conditions.
During austenite oxidation, Cu moves from the metal/oxide interface into the bulk of
the metal. Some of the remaining Cu-particles are entrapped inside the scale and
removed during descalling not being able to negatively affect the surface. In case of
oxidative conditions, decarburization takes place. The steadily decreasing austenite
grain is enriched in Cu enabling subsequently Cu precipitation in ferrite in a later
process stage. Precipitation of Cu-rich particles and Cu segregation along the grain
boundaries of ferrite is the root cause for grain degradation during hot rolling below
A3 and the creation of hot tears at the final TMR stages.
 7.1 Consideration regarding Cu precipitation Surface
Based on the oxidation process, the total iron mass that would form scale on a slab’s top quality of steel
surface can be calculated assuming that:
plates
(1) RH temperature is TRH ¼ 1,300oC with duration TRH ¼ 3 h; and
(2) the total initial Fe-Cu solution weights 100 g; subsequently Cu weights 0.4 g and
Fe 99.6 g. 221
The final solution after oxidation contains 0.4 g of Cu and these 0.4 g represent the
3 percent of the final weight.
Calling X the weight of the final solution, the final ferrite mass is calculated:
0.03X ¼ 0.4⩾x ¼ 13.3 g.
Consequently, from the 13.3 g of the remaining solution, still 0.4 g is Cu, so Fe in the
remaining solution is 12.9 g.
Concluding, in order to have minimum 3 percent Cu in the final solution, 87.05 percent
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of the initial Fe has to be oxidized:

(99.6-12.9)/99.6 ¼ 87.05 percent.
Indeed in the metal/scale interface ferritic grains can lose more than 80-90 percent of
their initial volume leading to Cu-rich particle precipitation (e.g. Figure 6).

7.2 Diffusion considerations

Supposing mild oxidizing conditions during RH, two phenomena take place in parallel:
first iron oxidizes in presence of oxygen forming FeO and second carbon diffuses from
the bulk metal to the atmosphere to form CO2 leading to decarburization of the surface.
Cu diffuses with the vacancy diffusion and C with interstitial diffusion. While the two
oxidation phenomena are parallel, their rates are different and independent. The carbon
oxidation reaction is faster, as it is defined by the carbon diffusion rate. As carbon is an
interstitial element in steel, at elevated temperatures it can diffuse to the oxidation
interface really quickly; this results in austenite poor in carbon, at a depth of certain
micrometers from the surface, which, when transformed, will only produce ferrite.
Ferrite presence is crucial for the Cu diffusion as according to the Fe-Cu binary diagram
it affects the overall solubility of Cu in ferrite. The solubility of Cu is reduced from
~8 wt-% in austenite to ~3 wt-% in ferrite according to Fe-Cu diagram. This practically
means that above 3 percent solid Cu will precipitate in ferrite.
During oxidation the volume of iron is continuously reduced due to scale
formation. As the steel/scale interface moves inwards, Cu diffuses to the grain
boundaries, and when the critical volume of 87.5 percent of the iron of the grain has
been oxidized, it precipitates in liquid form due to the temperature at the grain
boundaries. Liquid Cu penetrates the boundaries of the grains existing below the
interface in order to reduce the surface free energy, causing liquid metal embrittlement.
Additionally, the segregated liquid Cu at the boundaries diffuses back into the grains
enriching them even more. The mechanism involved in liquid Cu propagation
and hot shortness crack formation is best interpreted by Kirkendall void
formations, which are filled with liquid Cu. The above mechanism is given in detail
by (Fredriksson et al., 2001).
After the exit of the slab/billet from the reheating furnace (RF), temperature drops
rapidly in the surface during descaling, ferrite transforms from austenite in the surface
layer and Cu precipitates within ferrite.
 IJSI The effect of Si in Cu diffusion and hot shortness. Studies were carried out
6,2 to define how Si addition can affect hot shortness caused by Cu (Imai et al., 1997;
Seo et al., 1997a). It is suggested that Si addition up to 0.4 percent can reduce the
severity of hot shortness cracks as follows: Si causes internal oxidation in form of
globulitic oxides Fe2SiO4 (2FeO·SiO2 ¼ fayalite, e.g. in Jung et al., 2011), e.g. in Figure 2.
These oxides promote Cu occlusion in the scale instead of letting it stay at the steel-
222 scale interface, from where it would have the possibility of diffusing in the bulk
material, e.g. Figure 5(a),(e). The mechanism by which Cu is entrapped in the scale has
been proposed by Nicholson and Murrey (1965) Accordingly, Cu diffusion into the
grain boundaries is undermined by faylite-Cu-rich oxide particles, which are formed by
internal oxidation at the metal/scale interface. As oxidation proceeds Cu-rich oxides are
entrapped into the scale. Thus, Cu enrichment in the grain boundaries is limited.
Additionally, Si also suppresses the breakdown of scale facilitating its removal during
descaling prior to rolling.
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When entrapped in the scale, Cu can be removed without affecting the underlying
steel. In Seo et al. (1997a) it is also supported that Si increases the critical load that must
be applied on a steel workpiece with high Cu to fail from hot shortness. This is very
significant for the hot rolling process. Despite its positive impact in hot shortness,
special attention is required when increasing the Si content in steels as it is proven to
affect surface quality negatively.

7.3 Actions to avoid hot shortness issues

As oxidation conditions directly affect decarburization depth, one might consider
minimizing the relative oxygen pressure in the gas-furnace atmosphere during RH
without significant decrease in the decarburization depth. Lower oxygen atmosphere
decreases the rate of steel consumption and, thus, scale formation rate is also decreased,
while the diffusion rate of carbon remains high as it depends on temperature. This may
result in a wider decarburization zone as stated by (S.W.M., 2010).
An effective way to reduce oxidation and Cu segregation in the grain boundaries is
to reduce RH-temperature to 1,200oC and duration (no longer than 2-2.5 h). Reducing
RH temperature and duration a finer surface grain size will be also achieved,
which will affect positively Cu penetration (also according to findings of (Takemura
et al., 2011)).
As oxidation and diffusion are affected also by chemical composition, a decrease
in Mn (Ohtani et al., 1997) if possible (to maximum 1 wt-%), a reduction of Cu
(as low as possible; e.g. 0.1 wt-%) by scrap reclamation (Noro et al., 1997) and Si
additions of 0.3-0.4% might limit Cu diffusion into the grain boundaries and, thus, limit
surface liquid metal embrittlement with surface grain degradation during the final
forming stage.
For special steel and/or high quality steel production for automotive and
mechanical/engineering applications lowering the Cu level during EAF steelmaking is
achieved by DRI additions and usage of clean-shredded scrap. This is a more expensive
solution.

8. Conclusion
Diffusion related phenomena such as decarburization might cause additional problems
during steel products forming. It was shown that decarburization is the trigger to
extended Cu segregation within the surface layer Austenite grain boundaries. Prior to
 rolling, during descaling the austenite to ferrite transformation is accompanied by a Surface
drastic solubility reduction of Cu from ~8 wt-% to ~3 wt-%, respectively leading to quality of steel
Cu-rich particle precipitation at surface ferrite grains that are heavily oxidized
during RH even at Cu levels of 0.25-0.4 percent. Cu-rich particles on the surface cannot
plates
diffuse faster into the bulk metal than carbon migrates from the bulk to the surface
to be oxidized during decarburization (e.g. inside the reheating furnace – RF).
This practically means that the decarburization zone is likely thicker than the depth of 223
the Cu diffusion in the steel, considering the same exposure time.
Both Cu segregation and Cu-rich particle precipitation negatively affect surface
condition of bar/plate products and need to be avoided.
RF conditions (temperature, duration, atmosphere) and steel chemical composition
(e.g. C, Mn, Si levels) need to be carefully selected in order to facilitate Cu entrapment
within the scale so that it can be removed during descaling.
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Corresponding author
Dr Spyros Papaefthymiou can be contacted at: spapaefthymiou@elkeme.vionet.gr
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