Inclusion characterisation – tool for

measurement of steel cleanliness and process

control: Part 2
P. Kaushik*, H. Pielet and H. Yin
The research presented in this series of articles is a summary of inclusion characterisation
techniques in routine to support the process improvement needs of internal customers of
ArcelorMittal Global R&D, East Chicago. This paper highlights the use of characterisation
techniques including total oxygen analysis, cathodoluminescence microscope on remelt buttons
and clogging materials, and pulse discrimination analysis to study steelmaking and casting
issues that affect productivity and quality of steel at ArcelorMittal USA. Use of cathodolumines-
cence microscope for examination of remelt buttons to correlate the nature of inclusions to
castability for Ca treated steel grades is explained. Example results of application of total oxygen
analysis and pulse discrimination analysis on Ti stabilised ultra low carbon, advanced high
strength steels and transformation induced plasticity steels are shown. Formation of spinel
inclusions and their impact on castability for desulphurised non-Ca treated versus Ca treated
grades is also discussed.
Keywords: Cleanliness, Cathodoluminescence, Total oxygen, Pulse discrimination analysis, Ca treatment, Spinel inclusions

Introduction Sampling and experimental techniques

This article focuses on inclusion characterisation as a
unique tool to understand and resolve steelmaking and
casting issues that hamper productivity, yield and
quality of finished steel products. Part I1 reviewed steel
cleanliness measurement techniques in detail and
reported example results of inclusion analysis carried
out using an automated scanning electron microscope
(SEM). It was shown that the inclusion analysis results
from automated SEM helped in identifying issues such
as sources of non-metallics that deteriorate castability
and surface quality of Ti stabilised ultra low carbon
(TiSULC) grades, influence of steel chemistry on
clogging tendency of bake hardening grades, strong
steel slag emulsification for desulphurisation affecting
quality of advanced high strength steels (AHSS) grades
etc. In this article, use of techniques including total
oxygen OT, pulse discrimination analysis (PDA) and
cathodoluminescence microscope (CLM) will be shown
to study the dependence of inclusion chemistry and
morphology with process variability. Inclusion charac-
terisation was also used to study the role of spinels and
their influence on castability of Ca treated low carbon Al
killed (LCAK) steels.
Steelmaking and Casting Process Research, ArcelorMittal Global R&D,
Flat Carbon Americas, 3001 East Columbus Drive, East Chicago, IN, USA
*Corresponding author, email pallava.kaushik@arcelormittal.com
Sampling
Table 1 lists the chemistries of steel grades reported in
this paper. Table 2 outlines the process flow and
equipment used in the plants that produced these grades
and provided samples for characterisation. Chemical
and pin samples were collected as necessary to study a
particular production or quality issue.
The chemical samples were analysed for chemistry
using optical emission spectroscopy (OES). C and S in
tundish or mould samples were analysed using Leco.
Thereafter, the samples were cross-sectioned to obtain
portions to be analysed using two different techniques.
The samples were cut at the centre and mounted for
examination under an automated SEM as described in
the previous paper.1 A cylindrical pin was sliced from
the remaining cross-sectioned sample and remelted to
obtain a button. The remelted button was then
examined under cathode luminescence microscope
(CLM) and SEM to observe inclusion chemistry and
morphology. The chemical samples that contained
cavities either on the surface or inside were not used to
prepare remelt buttons. In addition, none of the
chemical samples was found fit for conducting OT
analysis.
Production pin samples were taken in some heats; a
portion was used to obtain OT information and the
remaining sample was used to prepare remelt buttons.
For the clogged nozzles supplied by the plants, the

ß 2009 Institute of Materials, Minerals and Mining

Published by Maney on behalf of the Institute
Received 28 March 2009; accepted 21 June 2009
572 DOI 10.1179/030192309X12492910938177 Ironmaking and Steelmaking 2009 VOL 36 NO 8
 Kaushik et al. Inclusion characterisation: Part 2

Table 1 Steel chemistries of different grades,* wt-%

Grade C Mn P Si Ti Al S N Ca

TiSULC 0.001–0.003 0.05–0.20 0.007–0.020 0.006–0.030 0.020–0.085 0.015–0.075 70–150 15–50 …

LCAK-1 0.035–0.055 0.20–0.30 0.030–0.070 0.020 0.003 0.040–0.070 50–80 40–60 7–18
LCAK-2 0.040–0.050 0.20 0.007 0.010 0.002 0.050 120 30–80 5–13
DP-AHSS 0.024–0.070 1.50–2.40 0.010 0.700 0.025 0.030–2.0 50 40–80 …
*S, Ca and N are reported in ppm; DP-AHSS refers to dual phase advanced high strength steels.

material was extracted from various cross-sections
across their length and mounted for CLM and SEM
examination. Energy dispersive spectroscopy was used
to obtain semiquantitative composition of the phases.
With the steel chemistries of the tundish samples,
thermodynamic calculations were made using Ceqcsi
software2 to compute equilibrium inclusion chemistry in
heats of LCAK-1 and LCAK-2 steel grades. The
thermodynamic results were compared with the results
of inclusion analysis in the samples.
Experimental techniques
Details about CLM technique were presented in the
previous publication.3 Cathodoluminescence is a cold
light phenomenon when non-metallic solids are bom-
barded with an electron beam. Since these solid particles
are usually luminescent with various colours under
CLM, different compositions and phases can be easily
identified by investigating the luminescence colour
images of these solids. The CLM is a combination of
an electron gun operated under low vacuum level
(y20 mBar) with an optical microscope at low magni-
fication (normally less than 6200). Under such condi-
tions, no sample preparation is required other than
simple degassing and dust/moisture removal. As the
observation field of the CLM is fairly large at lower
magnification, this allows rapid imaging of a big sample
to locate non-metallic features on its surface. The
cleaned sample is placed in the vacuum chamber
equipped with a manually controlled X–Y stage. The
electron beam is applied to the sample surface beneath a
lead glass window after degassing the chamber to a
prespecified vacuum level. The cathodoluminescence
colour emission generated by the electron beam excita-
tion is captured by a digital camera and stored for image
processing. During the startup of the CLM in April
2000, significant efforts were made to build a CLM
colour reference book to serve the needs of
ArcelorMittal R&D; a large number of reference
samples, samples from steel plants including pin samples
and nozzle clog materials and data from literature were
used to prepare this reference book.3
The applications of CLM in steelmaking research are
to locate inclusions on steel samples, identify castability
issues, study slag refractory reactions, and understand
mould flux reactivities. For example, the clogged
material from submerged entry nozzles is normally used
for ‘post-mortem’ identification of sources of clogging
by cross-sectioning and metallographic preparation of
the samples followed by their SEM examination.
Usually, the characterisation of these samples by SEM
analysis is a tedious and time consuming activity. In
contrast, visual examination of the samples under CLM
helps in perceiving a quick state of the heat and
identifying areas of interest to focus SEM characterisa-
tion work.
OT is the most widely used indicator for characterising
the cleanliness of a steel grade and for assessing process
improvements and quality control. It represents the sum
of oxygen soluble in liquid steel and present as oxide
inclusions. As the solubility of oxygen in liquid iron at
steelmaking temperatures is y4 ppm in Al killed steels,
OT can be considered as an indicator for the cleanliness
level of a heat. Measurement of OT is conducted by a
standard Leco testing procedure. Whereas this technique
has its own benefits including a quick and easy
assessment of cleanliness during various stages of
production, it is only applicable for oxide inclusions
and does not provide any information about inclusion
chemistry or morphology. Furthermore, contamination
with tundish or mould slag produces erroneous results.
Regardless, this technique is still useful in comparing
heats from different processes and plants, and can be
used in conjunction with the results of automated SEM
and CLM to examine the success of trials.
OES-PDA uses spark discrimination of the elemental
intensities present as the soluble element and in the
inclusions.4 Although this technique is faster than
automated SEM analysis and can be used with new
generation spectrometers, it does not provide informa-
tion about shape and size of the inclusions. In this study,
the broad face of chemical samples was analysed for
PDA using the same spectrometer that analysed
chemistry of steel, before cross-sectioning the samples
to carry out other analysis such as characterisation using
automated SEM. The algorithm to obtain PDA indices
is developed at ArcelorMittal Global R&D, Metz,
France. PDA was applied on certain samples to test its

Table 2 Plant and process flow to produce steel grades*

Secondary refining Steelmaking Caster Sample

Plant Grade equipment process flow mould location Type of sample

M1, M4 TiSULC RH-OB degasser BOF.stirring Vertical Tundish, mould Chemical, pin
station.degasser
M2 LCAK-1, LCAK-2, Ladle furnace BOF.ladle furnace Vertical, Ladle, tundish, mould Chemical, pin
DP-AHSS, TRIP Curved
M5 TiSULC Ladle furnace, BOF.ladle Curved Tundish, mould Pin
RH-KTB degasser furnace.degasser
*RH5 Ruhrstahl–Heraeus; OB5oxygen blowing; BOF5basic oxygen furnace; KTB5 Kawasaki top blowing.

Ironmaking and Steelmaking 2009 VOL 36 NO 8 573

Kaushik et al. Inclusion characterisation: Part 2
1 Image (CLM) of sample collected from clogged TiSULC
heat at plant M1: loose alumina structure (red) can be
seen; normalised clogging index (0?42) is also shown
potential use at USA plants for steel grades including
TiSULC and AHSS grades.
Results and discussion on techniques
Inclusion characterisation using CLM
Severity of nozzle clogging in TiSULC grades
The images shown in Figs. 1 and 2 compare the cross-
section of two nozzle clog samples from heats produced
at plant M1 during different cast sequences. The
corresponding clogging index is shown at top right in
each image, higher values indicating more plugging. As
seen, the severity of the clogging is also reflected in the
CLM images of the clogged mass. The density of the
mass as well as a first indication of the elemental
composition provides a quick idea about the relative
source of clogging before conducting detailed SEM
characterisation. For example, the heat shown in Fig. 1
has very few Ti containing alumina inclusions (blue
dots) in a pure alumina matrix (red) whereas Fig. 2
shows a dense alumina mass (red) and large quantity of
Titanium aluminates (blue particles). This indicates that
the sources (and likely mechanisms) of nozzle clogging
are different in these two heats. Quick location of non-
metallic particles in two different nozzle clog masses
using CLM helped in guiding the further characterisa-
tion work in SEM and reduced the time to report the
results by half. A study of steel characterisation by CLM
analysis of remelt buttons prepared from pin samples of
TiSULC grades was reported in a previous publication.5
Correlation of inclusions with castability of Ca treated LCAK
grades
In a study carried out to understand the effect of Ca
treatment on LCAK-1 and LCAK-2 steel grades, pin
samples were collected from the ladle, tundish, and
mould. Portions of the slabs from corresponding heats
were milled to obtain sections that were machined to
obtain pins. Remelt buttons were made from pin
samples and examined using CLM. Figure 3 shows the
CLM images of the inclusion rafts on the remelt buttons
from the tundish pin samples. The yellow material is
CaS and the green particles are liquid Ca aluminates, the
background being iron.
574 Ironmaking and Steelmaking 2009 VOL 36 NO
2 Image (CLM) of sample collected from clogged TiSULC
heat at plant M1 showing dense alumina mass (red)
and AlTi (light blue) inclusions: normalised clogging
index (0?84) is also shown
Previous studies at ArcelorMittal R&D had indicated
that inclusions on the remelt button rafts from success-
fully Ca treated Al killed heats appeared as molten pools
of liquid calcium aluminates in SEM images and as
brown ovals in CLM images. In contrast, the inclusions
on non-Ca treated Al killed heats had distinct faceted
and dendritic morphologies in SEM images5 and looked
red (pure alumina) or green (alumina with few percent
MgO) under CLM examination. Therefore, CLM
images were investigated to see if they could be used
directly to characterise the success of Ca treatment.
Expecting that CLM images of samples from poorly Ca
treated heats would exhibit red and green spots and few
or no round pools, the heats were ranked for castability
from 1 to 6, 1 being best and 6 being worst. The rankings
are marked at top left corner in the images shown in
Fig. 3. These rankings were plotted in Fig. 4 against the
castability index of the heats (defined as the normalised
average rate of change of the nozzle clogging factor). As
shown in Fig. 4, the visual rankings and the castability
index matched satisfactorily. The two heats with liquid
calcium aluminate inclusions (rankings 1 and 2) reduced
nozzle clogging significantly, as did one of the four heats
without liquid calcium aluminates (ranking 3) showing
that CLM imaging can be used to understand the
severity of nozzle clogging with respect to inclusion
types and compositions in Ca treated LCAK grades.
This indicates that CLM can be a faster tool for
characterising success of Ca treatment than detailed
SEM analysis.
AlN inclusions in high Al transformation induced plasticity
(TRIP) steel grades
High Al TRIP steels have a very good combination of
strength, formability and coatability. It is already being
used in automobile body design and will find a variety of
other weight reduction applications. However, lack of
knowledge of steelmaking and casting practices has
hindered their fast commercialisation. At ArcelorMittal
Global R&D, East Chicago, USA, enormous efforts
have been made to characterise these high Al steels
(.1%Al) to understand and optimise steel refining and
casting processes. It was found that the CLM analysis of
8
 Kaushik et al. Inclusion characterisation: Part 2

3 Images (CLM) of remelt buttons prepared from tundish pin samples of selected Ca treated LCAK-1 and LCAK-2 heats
produced at plant M2: rankings of heats from CLM imaging are shown at top left corner

both slab6 and mould pin samples7 can be a simple and
quick inclusion characterisation tool for these steel
grades. The dominant inclusions in these new steels are
1–5 mm AlN particles that fluoresce pure red under
CLM. Figure 5 is a CLM image of a mould pin sample
from a TRIP heat with about 1?1%Al and 40 ppm N.
The pure red clusters on the CLM image were all
crystalline AlN particles as confirmed by SEM energy
dispersive spectroscopy examination. A minority of
inclusions were spinels (green) and CaS (yellow). This
indicates that the previous knowledge on Al2O3 inclu-
sions in regular Al killed steels is not adequate to study
high Al TRIP steels. A new knowledge expertise needs to
be built for AlN inclusions in steels.
Cleanliness measurement using total oxygen
Cleanliness assessment of TiSULC grades over a period
The critical surface quality exposed TiSULC grades
produced at plant M1 are regularly monitored for
changes in product yield and sliver defects, similar to
other plants. As product downgrading and rejections
may not be entirely due to finishing defects, including
those generated from scarfing, rolling and galvanising
operations, the focus remains to measure and control
steelmaking defects. This calls for routine cleanliness
characterisation of heats produced in many cast
sequences to test the effects of changes in clean steel
practices in steelmaking and casting processes. As shown
in Fig. 6, OT has been used as an indicator to measure

Ironmaking and Steelmaking 2009 VOL 36 NO 8 575

Kaushik et al. Inclusion characterisation: Part 2

4 Variation of normalised castability index with rankings
of heats given from CLM images: higher value of cast-
ability index shows more plugging tendency of the
heat; all heats were Ca treated LCAK steels produced
at plant M2
6 Comparison of total oxygen in critical surface quality
exposed TiSULC steel grades produced at plant M1
from years 2000 and 2005

cleanliness over two different periods. Pin samples were

collected from the tundish well and the caster mould for
each strand multiple times during the course of casting
of the heats. The first heat on each cast sequence was
omitted from the analysis.
As seen in Fig. 6, the scatter in the difference between
OT measured in the tundish and in the mould is lower in
the study conducted in late 2005 than in studies
conducted before 2000. This data was also helpful in
identifying the possibility of any air entrainment during
casting when viewed in conjunction with N increase
from the tundish to the mould, found none from the
2005 data (not shown here). The average OT was
decreased by 7 ppm in the tundish during this period, 7 Total oxygen in TiSULC steel grades produced at plant
mainly ascribed to modifications in the steelmaking M5 to study impact of tundish furniture: three mould
practices including minimising the reducible oxide pin samples were collected for each heat; broken lines
content in the ladle sand, changing the ladle slag carry are drawn to show general trend
over detection system, improving tundish sealing prac-
tice and redesigning the tundish as part of the caster fluid flow patterns in the tundish (and dead zones)
mould conversion. A similar study was made to check contribute to inclusion separation and flotation leading
the possibility of steel reoxidation in the tundish by to improvement in cleanliness levels.8 An example is
collecting pin samples from the tundish pouring box and presented in Fig. 7 that show the reductions in OT when
the tundish well; the results indicated a linear relation- impact pads were used in the tundish for casting
ship between OT values measured at abovementioned TiSULC grades at plant M5. In this study, pin samples
locations suggesting tighter sealing at the tundish. were collected three different times during casting from
the caster mould of each strand for two cast sequences.
Impact of tundish furniture on TiSULC grades Nine heats were cast in each cast sequence. The sequence
The tundish furniture including dams, weirs and impact that did not use an impact pad served as the base case
pads act as distributors of liquid steel in the tundish. The for comparison.

5 a CLM and b SEM images of inclusion rafts on remelt button showing crystalline AlN particles on TRIP steel mould
pin sample

576 Ironmaking and Steelmaking 2009 VOL 36 NO 8


8 Relationship between oxide inclusion density in chemi-
cal samples versus total oxygen in pin samples col-
lected after completion of ladle furnace treatment for
AHSS grades produced at plant M2
As shown in Fig. 7, the OT levels were high during ladle
exchange, which continued to decrease as casting pro-
ceeded and reached y15 ppm when two thirds of the ladle
was drained. OT values of 20 ppm or lower can be
considered reasonable for cleaner TiSULC steels.9 With
an impact pad in the tundish, OT was found lower by an
average 3 ppm in most samples collected in middle of the
casting and up to 8 ppm in samples collected during ladle
exchange. The impact pad did not affect the cleanliness
levels for the first heats in the cast sequence, where the
effects of contamination from refractory coatings during
initial tundish fill, metal bath agitation and reoxidation
were more dominant. It becomes clear that the slag
emulsification at the ladle exchange has a large impact on
contamination of steel and that the specially designed
impact pads could reduce this contamination significantly.
This study helped justify the continued application of
impact pads in the tundish at plant M5.
Comparison between inclusion density and total oxygen for
AHSS grades
Comparison of OT with automated SEM inclusion
analysis is an important step to establish the usefulness
9 Al–O equilibrium and measured oxygen activity (open circles) from pin samples collected from TRIP heat
Kaushik et al. Inclusion characterisation: Part 2
of the automated SEM technique for process control.
Studies have shown that variations in OT and inclusion
indices have similar trends in a heat or a process.10,11
Figure 8 shows an example where OT is plotted against
the number density of oxide inclusions in ladle samples
collected for several AHSS grades from plant M2. The
OT was measured in the pin samples and the number
density of oxide inclusions was measured by an auto-
mated SEM on a cross-sectioned chemical sample. The
pin samples were collected by immersing a quartz tube
manually in the ladle close to the position where the
ladle production samples were collected using an auto-
matic pole to minimise variations in inclusions from
the fluid flow in the ladle.12 As shown in Fig. 8, a
higher OT corresponded to a higher density of oxide
inclusions in the ladle samples. This result provided a
direct confirmation that utilising the selected auto-
mated SEM analysis is a reliable tool for inclusion
characterisation for sophisticated AHSS grades.
Total oxygen in high Al TRIP grades
As mentioned in the previous section, high Al TRIP
steels contain AlN rather than Al2O3 inclusions. Before
production of these steels at plant M2, it was expected
that Al2O3 would be the major inclusion and would
cause nozzle clogging during casting. Conversely, to
everyone’s surprise, nozzle clogging did not occur even
after casting six heats in a production sequence of TRIP
steels. As shown in Fig. 5, the dominant inclusions were
AlN, but not Al2O3. Although a small amount of Mg
aluminate (spinel) inclusions accumulated in the vicinity
of the slide gate area during the cast,6 they did not affect
the clogging performance of the casting operation.
When OT analysis was made on the pin samples
collected from the caster mould, it was found that the
high Al TRIP steels are very clean in terms of oxide
inclusions; its OT is close to 5 ppm (average), which is
5 ppm lower than regular Al killed steels produced from
a similar steelmaking route in plant M2.
Thermodynamic analysis together with measurements
of oxygen activity in the ladle6 is reproduced here with
OT value for a heat containing 1?2% Al (Fig. 9). It can
Ironmaking and Steelmaking 2009 VOL 36 NO 8 577
Kaushik et al. Inclusion characterisation: Part 2
10 Comparison between normalised inclusion content
observed from automated SEM and PDA in chemical
and slab samples of DP-AHSS grades produced at
plant M2
be seen that the OT value is much lower than the
solubility of oxygen in high Al steel. When aluminium is
added to liquid steel, the Al–O reaction crosses the
lowest [O] point in Fig. 9 as Al increases beyond 0?2%
Al. At that moment, except for 2 ppm [O] dissolving in
steel, all extra oxygen will combine with [Al] to form
Al2O3 inclusions. Assuming that all Al2O3 formed can
be removed from steel, the OT will be the same as the
2 ppm soluble [O] even though the [O] solubility limit is
y10 ppm. In reality, the removal of Al2O3 inclusions
cannot be achieved completely and the remaining
alumina particles will start to dissolve into the liquid
steel once the [Al] exceeds the 0?2% threshold. Thus, the
OT in high Al steel will be at the valley value of 2 ppm
plus the [O] contributed from redissolved Al2O3 (Fig. 9),
or even a much lower value if most of the Al2O3
inclusions are removed from the liquid steel. As a result,
OT in high Al steels is much less than the equilibrium
solubility limit of [O].
Cleanliness measurement using pulse
discrimination analysis
Pulse discrimination analysis has been successfully used
in some plants in Europe for quick and online
assessment of inclusions on regular production samples,
including chemical samples and samples cross-sectioned
from slabs.4,13,14 Significant efforts were made at
ArcelorMittal Global R&D in Europe in the past to
develop a PDA algorithm to identify inclusions with
various chemistries. So far, the PDA is mostly applied
on ULC grades and Ca treated medium carbon grades.
In order to introduce this technology into the US for a
broader range of steel grades, a study was carried out on
a non-Ca treated AHSS steel grade produced at plant
M2. This work compared the inclusion content obtained
from PDA (analysed at ArcelorMittal Global R&D,
France) based on an algorithm developed on Ca treated
steels and from an automated SEM analysis.
The preliminary results are plotted in Fig. 10, in which
the relative proportion of alumina inclusions, Al–Mg
spinel inclusions and Al–Mg–Ca oxide particles is com-
pared in different samples collected along the production
route. As seen, the relative inclusion contents observed
using SEM in either sample differ significantly from that
acquired from PDA, specifically for inclusions containing
Al–Mg. In other words, although the trends of inclusion
578 Ironmaking and Steelmaking 2009 VOL 36 NO
chemistry variations had some similarity, particularly for
mould and slab samples, the PDA significantly under-
estimated the Al–Mg inclusions and overestimated both
pure alumina and Ca containing inclusions.
This inconsistency indicates the special need to develop
a new PDA element separation algorithm for the new
generation of AHSS steel grades with a different
steelmaking process. It is known that PDA can detect
inclusions larger than 2 mm and this could be one of the
reasons that caused the discrepancy. However, more
research is needed to better understand the PDA analysis
and use it for online application of inclusion engineering
needs for third generation AHSS grades. In addition,
while adopting this new technology for inclusion char-
acterisation, a detailed cross verification is always a good
idea such that the conclusions from the new technology
do not mislead the focus of process improvement.
Use of inclusion characterisation to
study spinel formation in Ca treated low
carbon Al killed steels
Magnesium aluminates (MgO.Al2O3) (popularly known
as spinels) have been shown to reduce castability of low
and medium carbon desulphurised and resulphurised
steels.15–25 Frank reviewed the formation and role of
spinels in liquid steels and their influence on the casting
process.15 The sources of MgO containing calcium
aluminate inclusions were reported to be lowering of
Ca content in the steel,16 contact time of liquid steel in
the ladles including contamination from ladle refrac-
tories,17,18 transfer from ladle slag,19,20 ladle glaze from
the previous heat21 and impurities from Al and
ferroalloys.22,23 A higher MgO content in the aluminate
inclusions has also been associated with accelerated
clogging during casting of these steels.15,16,20,24 Ca
treatment has improved the castability of LCAK steel
grades by formation of liquid Ca aluminates25,26 and by
modification of MgO containing alumina and spinel
inclusions.18,27
LCAK-1 and LCAK-2 heats were produced at plant
M2, differing mainly in sulphur and phosphorus
content, as shown in Table 1. After tapping from the
BOF, the heats were deslagged, followed by temperature
and chemical composition adjustment at the ladle
furnace. FeCa wire was added followed by a short rinse
in the ladle. Ca treated heats were cast in the middle of
the cast sequence whereas the non-Ca treated heats were
cast both at the beginning and during the cast sequence.
On non-Ca treated heats, tendency of plugging increased
as the casting progressed. During the trials pin samples
from ladle, tundish and mould were collected to prepare
remelt buttons for inclusion analysis using SEM, similar
to research reported previously.5,28 A portion of the
slabs was also cross-sectioned for inclusion characterisa-
tion using the remelt button technique.
From the SEM inclusion analysis of the remelt
buttons prepared from tundish pin samples, it was
found that non-Ca treated heats had a higher fraction of
pure alumina and 10–12%MgO containing aluminate
inclusions. For Ca treated heats, as expected, the
fraction of alumina inclusions was low with most of
the oxides being Ca aluminates containing about 18–
20%MgO. The inclusion chemistries, plotted as the ratio
of MgO to Alumina content, and their cumulative
8

11 Number and cumulative fraction of inclusions versus
MgO/Al2O3 ratio in remelt buttons of tundish samples
from non-Ca and Ca treated LCAK-1 heats produced
at plant M2
fraction for LCAK-1 and LCAK-2 heats are shown in
Figs. 11 and 12 respectively. The range for spinel
inclusions, MgO/Al2O3<0?24–0?42 is also marked. The
interpretation from these figures is that the desul-
phurised non-Ca treated LCAK-1 grades had larger
fraction of high MgO (y12%) containing alumina
inclusions while non-desulphurised non-Ca treated
LCAK-2 grades contained nearly pure alumina inclu-
sions with y6%MgO. While Ca treated heats of both
steel grades had more spinel inclusions than the non-Ca
treated heats. This led to the understanding that spinel
inclusions were not formed in the ladle treatment of
non-Ca treated heats but formed in Ca treated heats
during Ca wire injection. The likely reason for their
appearance in Ca treated heats seems to be due to
extended slag metal stirring and longer contact time with
alumina–magnesia–carbon refractories. This finding is
contrary to the observations by Garlick et al.17 where Ca
treated resulphurised Al killed steels had no spinel
inclusions in the tundish samples even with longer hold
times but were due to the residual Mg content in Al and
alloys added at tap. In the present study, some of both
non-Ca and Ca treated LCAK-1 heats were deoxidised
at tap using Al cones. A detailed analysis indicated no
13 Variation of MgO/Al2O3 in inclusions with product of MgO and Al2O3 in final ladle slag of non-Ca and Ca treated
LCAK steels produced at plant M2: spinel zone is also marked
Kaushik et al. Inclusion characterisation: Part 2
12 Number and cumulative fraction of inclusions versus
MgO/Al2O3 ratio in remelt buttons of tundish samples
from non-Ca and Ca treated LCAK-2 heats produced
at plant M2
statistical difference between spinel inclusion frequency
in the heats with or without Al addition at tap.
Furthermore, a significant Mg content in Al cones was
not reported. If the source of Mg was in Al, then both
non-Ca and Ca treated heats should have had a higher
(and similar) frequency of spinels which was not the
observation from inclusion analysis as shown in Figs. 11
and 12 strengthening the belief that extensive ladle
stirring for Ca treatment transferred Mg from slag and
refractory to the metal.
The solubility of Ca and Mg is reported to be low in
liquid steel,29 particularly the data on the solubility of
Mg content in steel is not in abundance. In this study, as
the chemical analysis of steel samples did not include Mg
content and due to uncertainties in the analysis and
measurement of Mg in steel, thermodynamic investiga-
tions were carried out using Ceqcsi software.2 The
calculations were carried out using the steel chemistries
measured in the tundish samples at 1550uC. The
calculation showed that Mg needs to be below
0?15 ppm to avoid precipitation of spinel inclusions in
non-Ca treated heats and y3?5 ppm for Ca treated
grades. This implies that at least 3 ppm Mg was
transferred from sources such as refractory and slag
Ironmaking and Steelmaking 2009 VOL 36 NO 8 579
Kaushik et al. Inclusion characterisation: Part 2
14 Variation of product of MgO and Al2O3 with sum of
FeO and MnO in final ladle slag of non-Ca and Ca
treated LCAK and TiSULC steels: heats that showed
spinels were all at FeOzMnO,1% (marked with
circles)
due to stirring carried out for Ca treatment. While there
existed a possibility of contamination of Mg from FeCa
wire, a mass balance calculation indicated that the
residual Mg in the FeCa wire had to be unreasonably
high to cause a 3 ppm Mg pick up by the liquid steel. As
reported,20,30 a lower oxygen activity would be needed
to form spinel inclusions. In the present study, the
oxygen activities calculated using Ceqcsi2 for the Ca
treated and non-Ca treated cases were 0?6 and 1?6 ppm
respectively.
Figure 13 plots the ratio of MgO to Al2O3 in the
inclusions versus the product of MgO and Al2O3 in the
ladle slag after completion of ladle treatment, called
16 Inclusion path in ladle, tundish, mould and slab samples of Ca treated LCAK heats produced at plant M2
580 Ironmaking and Steelmaking 2009 VOL 36 NO
15 Dependence of castability with inclusion composition
for non-Ca and Ca treated LCAK steels produced at
plant M2
M6A hereafter. As seen, there is no relationship
between inclusion content i.e. fraction of MgO with
M6A. Although the inclusion composition in Ca
treated heats indicated the presence of spinel particles
i.e. with MgO/Al2O3<0?24–0?42, the corresponding
M6A values varied from 255 to 330. Figure 14,
conversely, plots the M6A values against the sum of
ladle slag reducible oxide content for both TiSULC and
LCAK grades. As the sum of FeO and MnO decreased,
the values of M6A increased but not all LCAK heats
had spinels with higher M6A values (data within circles
in Fig. 14 are heats with spinels) and none of the
TiSULC heats produced at plant M4 with higher M6A
values contained spinel inclusions. The LCAK heats that
contained spinels had FeOzMnO ,1% but not all heats
8

with sum of FeO and MnO less than 1% showed spinels.
Ahlborg22 described a relationship between low oxida-
tion state of ladle slag with higher Ca–Mg aluminate
inclusion content in tundish samples, which were also
claimed for frequent clogging occurrences. In the present
study for LCAK steels, at low ladle slag FeOzMnO
contents, the MgO content of aluminate inclusions is
highly variable and the fraction of these inclusions is
high only in non-Ca treated heats, as estimated from
Figs. 11 and 12. Thus, the trend shown in Fig. 14
appears to be an effect of slag dilution due to slag
deoxidation, carried out using a mix of calcium
aluminate and Al, required for steel desulphurisation
for LCAK grades and for quality reasons in TiSULC
grades.
MgO containing inclusions, particularly spinels, have
frequently been reported to cause castability
issues;15,16,20,22,24 however in the present research, as
shown in Fig. 15, it appears that the MgO containing
aluminates and spinels did not increase clogging of
either Ca treated or non-Ca treated heats. Although the
Ca treated heats had better castability than non-Ca
treated heats, the variation of MgO/Al2O3 ratio was
similar in all inclusions other than spinels. It seems that
spinel inclusions that formed due to transfer of Mg from
slag due to extensive stirring during Ca injection were
modified to Ca–Mg aluminates by Ca treatment, in
agreement with Pistorius et al.,18 even though their
partial modification shows the inclusion composition
(expressed as MgO/Al2O3 ratio) to fall in spinel range.
As spinels do not agglomerate in comparison to
alumina, their relationship with poor steel castability
seems to depend on other process variables.
The inclusion composition observed in samples
collected from ladle, tundish, mould and slabs in Ca
treated LCAK heats is shown in Fig. 16. At the
completion of ladle treatment, mostly alumina and high
MgO containing aluminate inclusions were present that
changed to Ca–Mg aluminates in tundish followed by
liquid Ca aluminates in mould and slab samples. More
scatter in inclusion chemistry was present in the tundish
and the slab samples, compared to the ladle samples.
The transformation of Ca–Mg aluminates to liquid Ca
aluminates in mould samples explains why Ca treated
heats did not plug as much as non-Ca treated heats.
Summary and conclusions
This article has summarised the inclusion characterisa-
tion methods using remelt buttons and cathodolumines-
cence, pulse discrimination analysis and total oxygen to
support the process improvement needs of internal
customers of ArcelorMittal Global R&D, East
Chicago. The major conclusions from this research are
as follows.
Evaluation of techniques
The techniques that were employed for inclusion
analysis were cathodoluminescence microscopy on
remelt buttons and nozzle clog materials, total oxygen
analysis on pin samples, automated and operator
assisted SEM and pulse discrimination analysis on
chemical samples of TiSULC steels, LCAK steels,
AHSS and TRIP steel grades produced at various
plants. The conclusions related to automated SEM
Kaushik et al. Inclusion characterisation: Part 2
technique were presented in Part I of this series of
articles.1
1. Inclusion composition in nozzle clog material and
remelt buttons can be quickly perceived using CLM.
More importantly, from comparison of inclusion
composition and size among different heats, the
source/origin of the casting issue can be easily
identified. For example, the severity of the nozzle
clogging in Ca treated LCAK grades was correlated
to visual ratings of CLM images, based on inclusion
chemistry and morphology. Moreover, examination
under CLM helps a user to select portions of the
clog mass or raft on the remelted surface to guide
the inclusion analysis to be conducted with operator
assisted SEM.
2. OT is used as indicator to assess steel cleanliness as
appropriate. This technique is helpful in assessing
the effectiveness of continuing trials or applications
of new devices to improve secondary refining and
casting process. In this study, it served as a quick
tool to measure cleanliness levels for critical
TiSULC steel grades produced over different
periods to predict the impact on quality. A good
relationship was found between oxide cleanliness
measured using OT and inclusion density measured
from automated SEM analysis on AHSS grades.
3. PDA can be used for online assessment of inclusion
content and composition to evaluate the success of
trials oriented towards process monitoring and
modification of clean steel practices. When used
for DP-AHSS grades, the results of normalised
inclusion contents from PDA and SEM analysis
differed. Whereas it has been successfully used for
TiSULC and Ca treated steel grades, future research
is needed for its application for third generation
AHSS grades.
Thus to comment on suitability of each technique, total
oxygen measurement is a standardised procedure, the
results of which can be compared with historical and
published data. PDA is a developing technique that is
expected to be useful for quality control when changes
from standard practices result in significant variation in
inclusion indices. Remelt buttons used with CLM is an
important technique, unique to ArcelorMittal, for
process diagnosis and improvement since it provides
rapid overview of large number of inclusions.
Automated SEM is useful for in-depth study of effect
of processing on inclusion size, chemistry and distribu-
tion. For Ca treated LCAK steel grades, observation of
remelt buttons under CLM is a preferred method.
Steelmaking findings
Based on the inclusion characterisation, the following
observations were drawn for steelmaking practices that
helped to improve quality of steel.
1. Using OT, the influence of open eye around ladle
shroud during casting and application of tundish
furniture was evaluated. The results verified the
importance of minimising steel reoxidation in
the tundish during ladle exchange that affects the
inclusion population and composition.
2. Ca–Mg aluminate inclusions were observed in both
non-Ca treated and Ca treated LCAK steel grades;
inclusions with compositions close to pure spinels
were in higher frequency in Ca treated heats. It is
believed that Mg transfer from slag metal stirring
Ironmaking and Steelmaking 2009 VOL 36 NO 8 581
Kaushik et al. Inclusion characterisation: Part 2
and contamination from refractory due to extended
stirring during and after Ca treatment led to this
observation. There was no indication of poor
castability of Ca treated heats due to the presence
of spinel or MgO rich aluminate inclusions.
3. AlN, and not Al2O3, are major inclusions in high Al
TRIP steels. Additionally, these steels were much
cleaner as OT was 5 ppm, lower than in the regular
Al killed steels that helped explained good cast-
ability of these TRIP steels.
In conclusion, inclusion engineering requires tools such
as thermodynamics, industrial process data, and results
from mechanical tests on products to evaluate the
metallurgical benefit of process and quality control.
Visual and quantitative characterisation of inclusions
enhances understanding for process modifications. The
techniques outlined in these papers are used as appro-
priate to address quality or production concerns in
secondary steelmaking and casting processes. Inclusion
characterisation activities will continue to help improve
the operations and to develop a quality monitoring
system.
Acknowledgements
They authors acknowledge the help of N. Jin, L. Keippel
and S. Schuldt for remelt button preparation and
chemical analysis of the samples. They express their
thanks to R&D technicians L. Laus, J. Thacker and P.
Martin in sample preparation and examination in CLM
and SEM. Discussions with D. Kruse on this piece of
research is deeply appreciated.
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