AISTech 2019 — Proceedings of the Iron & Steel Technology Conference

6–9 May 2019, Pittsburgh, Pa., USA

DOI 10.1000.377.221

Growth Mechanism of Clog Materials in SEN During Continuous Casting of Ti-Added ULC Steel

Joo-Hyeok Lee1, Sung-Kwang Kim2, Myeong-Hun Kang2, Youn-Bae Kang1,3

1
Pohang University of Science and Technology
Pohang, Rep. of Korea, 37673
Phone: +82-54-279-9032
Email: ybkang@postech.ac.kr
2
POSCO
Gwangyang, Rep. of Korea, 57807
3
Polytechnique Montreal
Montreal, Canada, H3C 3A7

Keywords: Ti-ULC Steel, Continuous Casting, Nozzle Clogging, Oxidation

INTRODUCTION
Clogging of Submerged Entry Nozzle (SEN) during continuous casting of liquid steel has been an important issue both in
productivity and product quality control. Severe nozzle clogging causes an unstable fluid condition in a mold due to out of
control of the flow control device (e.g., stopper or slide gate), a decrease of net casting throughput due to decreased passage
volume of liquid steel, quality degradation of cast slab and rolled sheet product due to dislodged clog. Although numerous
investigations were carried out to understand these phenomena and to find countermeasures, it is still not well understood due
to complexities in the origin of the phenomena [e.g., 1]. Clog materials are reported in various forms of various kinds of
chemicals [2]. One of the most typical clog materials is clustered alumina well attached inner wall of SEN [3,4].
When Ultra Low C (ULC) steel is cast, the extent of the clogging becomes more serious. Adding Ti in ULC steel makes the
situation worse. Severe nozzle clogging by increasing Ti content in ULC steel has been reported [5-7]. The typical shape of
the clog in Ti-ULC casting SEN is a mixture of frozen skull with alumina. Increasing Ti content up to a few hundred mass
ppm changes the nozzle clogging phenomena considerably. Table 1 shows a summary of the possible cause of the severe
nozzle clogging by Ti addition. Although a flow characteristic of liquid steel in a tundish to mold may be responsible to a
nozzle clogging, it is hard to understand that Ti addition up to a few hundred ppm in RH would affect the flow characteristic
of the liquid steel. On the other hand, its physicochemical effect may be given further consideration.
There have been a number of reports that adding FeTi alloy in the ULC steel changes non-metallic inclusion evolution in the
liquid steel [8-12]. Although the most probable cause of nozzle clogging is usually adhesion of non-metallic inclusions, it is
still not clear why the increase of Ti content affect the nozzle clogging while stable inclusion phase is still alumina. It still
needs further investigations on inclusion evolution and its consequences on nozzle clogging for the case of Ti-ULC steel.
The present authors recently pointed out that the increase of Ti content up to a few hundred ppm may play an important role
in interfacial phenomena between liquid steel and the SEN refractory [7,13,14]. It was stressed that chemical condition at the
interface between the liquid steel and the SEN refractory would not be the same as that in the bulk steel. Most different
condition at the interface is oxygen potential that may cause a serious reoxidation of the liquid steel, thereby forming a
different intermediate phase than usual alumina clusters. This is because a carbothermic reaction inside the SEN refractory
produces a CO gas. This causes an excessive reoxidation of the liquid steel at the interface. Interestingly, the reoxidation
phenomena under the CO gas was dissimilar between Ti-free ULC steel and Ti-ULC steel [7,13]. Details phenomena of the
reoxidation by CO gas can be found elsewhere [7,13], and briefly summarized in the present article. Furthermore,
conventional use of Ar gas in tundish stopper may also bring a source of reoxidation due to a trace of oxygen in the Ar gas.
In the present article, the growth of the clog material in Ti-ULC steel continuous casting is considered as a result of
interfacial reoxidation reaction between the Ti-ULC steel and gas containing oxidation source. First, an interfacial
reoxidation of Ti-free Al-killed steel by the carbothermic reaction in SEN refractory is introduced. Then, a different

© 2019 by the Association for Iron & Steel Technology. 2147

reoxidation behavior of Ti-ULC steel by CO gas due to the carbothermic reaction is shown from the present authors’ recent
report [7,13]. Finally, an extension of the reoxidation study by employing different grade of Ar gas is reported in the present
study based on thermodynamic analysis and laboratory scale experiment.

Table 1. The possible role of Ti addition to ULC steel on SEN clogging during continuous casting.

Possible cause Comment

Reoxidation through nozzle refractory
or connector to slide gate/tundish
Adhesion of suspending inclusions to
an inner wall of the nozzle
Decreasing surface/interface tension of
liquid steel
Chemical reactions between nozzle
refractory and liquid steel
Solidification of liquid steel on nozzle
inner wall
Precipitation of alumina near nozzle
inner wall due to heat transfer
Clogging is observed to be severe below meniscus level and near the exit
port.
Ti may affect inclusion evolution, followed by attaching to the inner
wall of the nozzle [8-12].
Ti may lower the surface/interfacial tension of the liquid steel,
followed by enhanced wetting to the inner wall of the nozzle [15,16].
Ti-containing materials would form at the interface [7,13,17].
Solidification temperature of the steel by adding < ~0.1 Ti decreases only
~2 °C.
Ti is hardly responsible for the precipitation of alumina.

INTERFACIAL REACTION BETWEEN AL-KILLED STEEL AND NOZZLE REFRACTORY

SEN refractory is typically composed of a number of oxide component (SiO2, Al2O3, ZrO2, CaO, etc.), C, binder, and anti-
oxidant. During a casting operation, an increasing temperature inside the refractory results in a series of carbothermic
reaction. SiO2 is typically reduced by C:

SiO2(s) + C(s) = SiO(g) + CO(g) (1)

or
SiO2(s) + 3C(s) = SiC(s) + 2CO(g) (2)

It was also reported that Al2O3 can be also reduced by C:

Al2O3(s) + 2C(s) = Al2O(g) + 2CO(g) (3)

All of these reactions generate CO(g) that can propagate through pores in the refractory toward the interface between the
refractory and liquid steel passing through the SEN. The CO(g) then oxidizes Al in the liquid steel:

2Al + 3CO(g) = Al2O3(s) + 3C (4)

The generated Al2O3(s) is called network alumina, and it plays as a favorable site for suspending alumina inclusion in the
steel stream to adhere easily. By this mechanism, the alumina can build up inside the SEN and causes the nozzle clogging.
Different size and shape between the network alumina and the build-up alumina can be seen [18]. A schematic figure for the
above mechanism is shown in Figure 1 [19].

INTERFACIAL REACTION BETWEEN TI-ULC STEEL AND NOZZLE REFRACTORY

Unlike Figure 1, the clog material often observed after the Ti-ULC steel continuous casting is composed of frozen steel
mixed with non-metallic inclusions [5,6,14]. As listed in Table 1, increasing Ti content up to just a few hundred ppm would
not change the solidification character of the steel (solidification starting temperature only decreases no more than 2 °C).
A recent investigation by the present authors showed that Ti-ULC steel reacted with CO gas resulted in a mixture of solid
alumina and liquid oxide that consists of FetO-Al2O3-TiOx. Figure 2 shows the surface of the Ti-ULC steel sample oxidized

2148 © 2019 by the Association for Iron & Steel Technology.

by CO gas at 1560 °C [7]. SEM-EDS analysis revealed that not only Al2O3 but also a complex oxide composed of FetO-
Al2O3-TiOx (hereafter called FAT). According to the phase diagram analysis, the FAT was a “liquid” phase at the
temperature. This oxidation reaction was simulating the interfacial phenomena between Ti-ULC steel and CO gas which was
produced by the carbothermic reactions in SEN refractory produced (Reactions (1) to (3)). The oxidation condition is similar
to that shown in Figure 1. However, not only Al but also Ti and Fe were simultaneously oxidized.

Figure 1. Adhesion mechanism of alumina inclusions on SEN surface [19].

(b)
FetO-Al2O3-TiOx
Fe-0.0125Al-0.05Ti
(a)

Al2O3
10 µm
(c) Al (d) Ti

1 mm
(e) Fe (f) O

Figure 2. Observations for Fe-0.0125Al-0.05Ti sample after the reaction with CO gas: (a) visual appearance, (b) SEM image
of surface of the sample, and EDS mapping data for (c) Al, (d) Ti, (e) Fe, and (f) O, respectively [7].
Figure 3 shows an oxide stability diagram of Fe-Al-Ti-O system [20]. This oxide stability diagram puts an emphasis on
looking at low Al, low Ti region (high O content) in the diagram, contrary to the previous concerns to bulk composition. Due
to the oxidation by CO gas at the interface, local composition of the Ti-ULC steel changes from its bulk composition
(alumina as a stable oxide phase) to a region of low Al, Ti content, where the liquid oxide (FAT) becomes stable.
Since the FAT contains a substantial fraction of FetO, it is thought that the liquid FAT easily adheres to the alumina, the
liquid steel, and the SEN refractory. Based on this finding, a possible mechanism of clog material formation was proposed
[7]. It is shown schematically in Figure 4.

© 2019 by the Association for Iron & Steel Technology. 2149

 Fe-Al-Ti-O
0 5 (Ti,Al)2 O3
1540°C 6

-1 6
7

10 (Ti,Fe)3O5

log [mass pct Ti]

-2 Ti-ULC (bulk)
20
30

-3 50 Ti-ULC (interface)
100 Al2O3
-4 (FetO-TiOx
-Al2O3) 200 50 30 20 10 5 3 6
500
-5
1000

-6
-6 -5 -4 -3 -2 -1 0
FeAl2O4 log [mass pct Al]

Figure 3. Oxide stability diagram of Fe-Al-Ti-O system at 1540 °C reported by Kang and Lee [20]. Bold-italic numbers
stand for O concentration in liquid steel.

Figure 4. A schematic mechanism for nozzle clogging during continuous casting of Ti-ULC steels proposed by Lee et al. [7].

INTERFACIAL REACTION BETWEEN TI-ULC STEEL AND AR GAS INJECTED

During the continuous casting of liquid steel, Ar gas is often injected from the upper nozzle into the SEN in order to prevent
nozzle clogging. It is believed that a curtain of Ar gas forms and surrounds the liquid passing through the SEN [21]. This Ar
gas physically separates the liquid from contacting the inner wall of the SEN, thereby lowering the possibility of clogging.
However, it is also concerned that cleanliness of the Ar gas may influence the surface oxidation of the liquid steel.

2150 © 2019 by the Association for Iron & Steel Technology.

Figure 5 shows a calculated diagram of Fe-Al-Ti-O system showing thermodynamically stable phases at different oxygen
partial pressure and Ti content in the steel at 1540 °C. Al content was set to 0.025 %. The thermodynamic calculation was
carried out using FactSage [22] with FTmisc for liquid steel (Liquid), FTOxid for solid oxides (Al2O3, Ti3O5, Fe3O4,
Fe(Al,Ti)2O4), and a private database for the liquid oxide (FAT) [20]. Obviously, the liquid steel is stable at low oxygen
partial pressure, but it is oxidized by increasing the oxygen partial pressure. If an Ar gas with a certain level of oxygen as an
impurity, then the oxygen can oxidize the surface of the liquid steel. Depending on the oxygen partial pressure and the Ti
content, various oxides can form. In order to validate this thermodynamic analysis, a laboratory scale experiment was carried
out.

Fe - 0.025Al - xTi, T = 1540 °C

0

FAT(FetO rich) + Fe3O4

-4 FAT(FetO rich)
Normal Ar
(PO2 = ~ 10-6)
Liquid + FAT(FetO rich)
log PO2 (bar)

-8 + Fe(Al,Ti)2O4

Liquid + FAT(FetO rich)

Liquid + Al2O3 + FAT(FetO rich)
-12
Liquid + Al2O3 + Ti3O5

Liquid + Al2O3
-16
Liquid
Clean Ar
(PO2 = ~ 10-18)
-20
0 0.02 0.04 0.06 0.08 0.1
Mass percent Ti

Figure 5. A calculated diagram showing stable phases after oxidation of Fe-0.0025%Al-x%Ti alloy at 1540 °C using
FactSage [20,22]. “FAT” stands for liquid oxide composed of FetO-Al2O3-TiOx.

Experimental procedure
The experimental method used in the present study is almost identical to that used in the previous study [7] where CO gas
was used as an oxidation gas.
Approximately 0.5 kg of electrolytic iron was melted at 1600 °C in a MgO crucible using an induction melting furnace. O
preexist in the iron as an impurity was removed as much as possible by flowing Ar-4 pct H2 gas mixture during the melting.
By adding an appropriate amount of Ti sponge (99.9 mass pct., Kojundo, Japan) and/or Al pellet (5N grade, Kojundo, Japan)
into the molten iron after lowering the O concentration, a master alloy of Fe-0.025Al-0.05Ti was prepared. After
homogenizing, samples were obtained by quarts tubes of 4 × 10-3 m inner diameter to obtain bars of the sample. The surface
of the samples was ground to remove any oxide film, before subsequent oxidation experiment.
The sample was placed in a shallow alumina crucible, which was put in a quartz tube equipped with an RF generator (40 kW,
260 kHz). The tube was sealed by end caps in order to control the atmospheric condition. Two oxidation experiments were
carried out: melting the sample under clean Ar gas or under normal Ar gas. The normal Ar gas was 6N grade (99.9999%
purity). This normal Ar gas was used in one oxidation experiment without any purifying step. In the other experiment, the
normal Ar gas was purified by passing through CaSO4 column, and MgO chips at 550 °C flowed at 0.5 L min-1 through an
inner quartz tube. Power of the RF generator was adjusted in order to set a temperature at 1560 °C, which is 20 °C higher
than that used in Figure 5 in order to ensure melting of the sample. During the experiment, the oxygen partial pressure of
outlet gas was monitored by an oxygen sensor. The oxygen partial pressure of the normal Ar gas was ~ 10-6 bar, while that of
the clean Ar gas was ~ 10-18 bar, respectively. After 30 minutes, the power was turned off in order to quench the sample.
The surface of the samples was analyzed using Scanning Electron Microscopy (SEM) with Energy Dispersive Spectrometry
(EDS).

© 2019 by the Association for Iron & Steel Technology. 2151

Experimental results
Figure 6 shows photographs of the two samples reacted with normal Ar gas (Figure 6(a)) and clean Ar gas (Figure 6(b)),
respectively. By an eye inspection, it can be easily seen that one sample oxidized by the normal Ar gas is covered by some
oxides, while the other sample reacted with the clean Ar gas looks shiny on its surface. The surface of these two samples
were observed using SEM. Shown in Figure 7 is a BSE image of the sample oxidized by the normal Ar gas and EDS
elemental mapping for Fe, Al, Ti, and O. It is clearly seen that the surface is almost completely oxidized. Over all the area,
strong O peak was detected. As marked in the BSE image, three different regions were observed: FAT, Al2O3-TiOx, and
Al2O3, respectively. Average composition in each phase was measured by EDS, and these are shown in the inserted table.
This phenomenon is somewhat similar to the result reported in the present authors' previous study using CO gas, instead of
Ar gas.

Fe-0.025Al-0.05Ti

Normal Ar Clean Ar
(PO2 = ~ 10-6) (PO2 = ~ 10-18)

(a) 2 mm
(b) 2 mm

Figure 6. Surface of steel sample (Fe-0.025%Al-0.05%Ti) oxidized at 1560 °C under a) PO2 = 10-6, b) PO2 = 10-18.

Surface Fe Ti Al O
(2) Al2O3-TiOx

(1) FAT

wt.% Fe Al Ti O
(3)Al2O3 (1) FAT 50.27±5.17 3.00±0.68 15.92±1.83 30.82±2.76

10 µm (2) FAT (low FetO) 3.75±1.38 14.09±2.71 28.58±1.68 53.58±0.67

(3) Al2O3 1.79±0.61 44.06±1.70 0.81±0.28 53.34±2.45

Figure 7. SEM-EDS analysis results of the sample in Figure 6(a).

On the other hand, the other sample reacted with the clean Ar gas was not oxidized indeed. Any noticeable oxide phase
could not be found during the SEM-EDS analysis. These observations on the surface look to be consistent with the
thermodynamic analysis shown in Figure 5. In the present authors’ previous investigation using CO gas, a pure Fe (prepared
from electrolytic Fe) was not oxidized by the CO gas, while other samples containing Al only, Ti only, Al and Ti together
were all oxidized [7]. In the present study, the sample containing Al and Ti together was oxidized under the normal Ar gas
(high oxygen partial pressure), while the other sample of the same composition was not oxidized under the clean Ar gas (low
oxygen partial pressure). Therefore, it can be concluded that surface oxidation of Fe-Al-Ti alloy is governed by the alloy
composition and the oxygen partial pressure. And Ti-ULC steel usually contains Al and Ti to a few hundred ppm, both, its
reoxidation at the interface is dependent on the oxygen partial pressure at the interface.

2152 © 2019 by the Association for Iron & Steel Technology.

 DISCUSSION
Formation of intermediate oxide (FAT + alumina)
When liquid steel passes through a SEN, the steel is inevitably contacting the inner wall of the SEN. If the steel contains a
substantial amount of suspending inclusion such as alumina, then the alumina adheres to the inner wall, and the nozzle
becomes clogged. This type of clogging has been suppressed by improving the cleanliness of the liquid steel (removal of the
inclusions before the steel comes into a tundish) or by lining the inner wall with lime containing materials [1].
According to the network alumina formation mechanism shown in Figure 1 [19], the growth of an initial clog material seems
not dependent on the amount of suspending alumina in the bulk liquid steel. Inherent carbothermic reaction inside the SEN is
partly responsible for the initial growth of the clog material, through the Reactions (1) to (4). This is the case when the liquid
steel contains Al, but low C and low Ti. The initial clog material is alumina by the reoxidation due to CO gas. The bottom
part of Figure 3 may explain the stable clog material in a low C – Al-killed steel.
When the Ti-ULC steel is considered, bulk composition of the steel may be said to be a few hundred ppm of Al and Ti,
respectively, and a few tens ppm of O (~ 10 to 20 ppm). According to Figure 3, the bulk condition falls in an alumina stable
region. However, continuously produced CO gas or injected Ar gas of low cleanliness (containing oxygen as an impurity)
can reoxidize surface of the liquid steel at the interface between the steel and the nozzle refractory. And contrary to the case
of Al only killed steel, the reoxidation of Ti-ULC steel results in the formation of liquid FAT oxide mixed with solid
alumina. This changes the wettability of the liquid steel toward the inner wall of the refractory significantly.
Bernhard et al. reported that a contact angle between Fe-Ti alloy and solid alumina substrate in the temperature range of 1550
°C to 1620 °C decreased significantly when an intermediate layer was formed between the alloy and the substrate as a result
of a reactive wetting [17]. Although detailed reaction was not revealed, it was inferred that a less stable ceramic as the
substrate might be a reason for the reactive wetting followed by the formation of the intermediate layer, consequently
resulting in the decreasing the contact angle. The intermediate layer was found to be FeAl2O4 for low Ti alloy but Ti content
in the layer increased as Ti content in the alloy increased. According to the report of the present authors [7, 22], the Ti oxide
containing intermediate layer would be a liquid oxide that simultaneously contains FetO and Al2O3. Therefore, it is likely
that the formation of the intermediate layer between SEN refractory and Ti-ULC steel increases adhesion among the liquid
steel, alumina, and the SEN.

Role of the FAT in the growth of clog material

Once FAT forms along with the alumina, it adheres to the refractory and also contacts with the liquid steel. Since the steel
contains Al and Ti together, then these can reduce the FetO component in the FAT at the other interface between the FAT and
the liquid steel. As a result, a mixture of reduced Fe and TiOx-Al2O3 originally from the FAT, along with solid alumina can
be seen in the clog material. This possibility was proposed in the present authors’ previous publication [7] and is
schematically shown in Figure 4. It is now validated by a series of separate experiments. The results will be available
elsewhere [23].

CONCLUSIONS
A growth mechanism of clog materials in SEN for continuous casting of Ti-ULC steel was investigated by thermodynamic
analysis and laboratory scale experiments. Following the previous investigation regarding reoxidation of Ti-ULC steel by
CO gas that is generated inside SEN refractory, a reoxidation of Ti-ULC steel by a trace of oxygen in Ar gas was
investigated. It was shown by the experiment and the thermodynamic analysis that cleanliness of the Ar gas which is usually
injected in the SEN may affect the reoxidation of the liquid steel. The reoxidation (both by CO and by Ar containing O as
impurity) caused a formation of a mixture of solid alumina and liquid oxide composed of FetO-Al2O3-TiOx. The latter
influences wettability among various materials at the interface between SEN and the liquid steel, resulting in tight contact
among them. This is considered to be an initial growth mechanism of the clog material in the SEN for the Ti-ULC steel
continuous casting.

ACKNOWLEDGEMENT
This research was financially supported by POSCO.

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2154 © 2019 by the Association for Iron & Steel Technology.