Detection of NMI in Steel
Detection of NMI in Steel
Detection of NMI in Steel
Casting Billets
YING REN, YUFENG WANG, SHUSEN LI, LIFENG ZHANG, XIANGJUN ZUO,
SIMON N. LEKAKH, and KENT PEASLEE
This work applied automated particle analysis to study non-metallic inclusions in steel. Com-
pared with traditional methods, the approach has the advantage of capturing the morphology,
measuring the size, recording the original positions, and identifying the composition of inclu-
sions on a selected area in a short time. The morphology and composition of typical inclusions
were analyzed using partial acid extraction and discussed through thermodynamic calculation.
Steel samples were collected from the entire cross section of billets cast during times of steady
state and ladle change. The spatial distribution of inclusions agreed well with the measurement
of the total oxygen. The spatial distribution of inclusions was plotted to represent the entrap-
ment positions of inclusions on the casting strand and their concentration on the cross section of
the billet. Also, regarding the different size and type of inclusions, the spatial distribution of
classified inclusions was explored such as the distribution of sulfide, oxide, and high sodium and
potassium content inclusions. The sufficient information could be used to identify the source of
inclusions and guide the steel refining process.
DOI: 10.1007/s11663-014-0042-y
The Minerals, Metals & Materials Society and ASM International 2014
C Si Mn S Ti Mg Al Ca
0.20 0.23 0.48 0.006 0.002 0.0006 0.011 0.0002
II. METHODOLOGY
A. Experimental Procedures
Billet samples were obtained from an industrial plant
casting aluminum-killed medium carbon steel in a four
strand, 150 9 150 mm2 billet caster. The composition of Fig. 1—Sampling from a steel billet.
the steel produced is given in Table I. The tundish was
lined with refractory material high in magnesium oxide observation of inclusions was performed using an
with vertical straight nozzles submerged 100 mm below automated SEM–EDS—ASPEX 1020 system.[27]. The
the meniscus of the mold. The casting speed was 1.5 to automated particle analysis is a frame-based analysis.
2.0 m/min resulting in a standard casting time of about First, a selected area was divided into several small fields
45 minutes per heat with 2 to 3 minutes required to under the microscope. A focused electron beam was
change a ladle. A casting sequence typically pours 4 to 6 positioned on one field, and the microscope did a fast
heats with 60 ton per heat, depending on the lifetime of search of the field with large search steps. The intensity
the submerged entry nozzle and the casting schedule. of the back-scatter electrons was then recorded and
Billets samples were collected at both steady state and transferred to a computer. Once a particle was found
unsteady state. One sample was taken from the second based on thresholding of the intensity of the back-
strand of the billet caster after 3 heats of pouring at a scatter electrons, the step size was reduced to measure
casting speed of 1.5 to 1.7 m/min to represent the more precisely the dimensions of the particle. The center
steady-state (S1) operation. Another sample was of the particle was identified using a bisected chord
obtained during ladle change to reflect the unsteady method, and the rotating chord algorithm was employed
state of the casting process (S2). These samples were cut to measure the particle. Finally, the beam was again
into sections, as shown in Figure 1. A billet sec- positioned in the center of the particle to acquire the
tion 5 mm in thickness was used for oxygen analysis characteristic X-ray. After combination of these steps in
to map the three-dimensional distribution of oxide one field, the beam moved to other fields and repeated
inclusions over the billet cross section. the analysis.[28,29]
For the oxygen samples, a 5-mm-thick billet slice was In the present study, using ASPEX 1020 system, the
sawed into 45 rectangle samples with the dimension of size distribution, composition, and rough morphology
30 9 15 9 5 mm3, as shown in Figure 2(a). Each sam- are automatically obtained. Although the images of
ple was machined into three cylindrical samples, with a inclusions obtained using ASPEX are not high in
diameter of 5 mm for the oxygen analyzer. For the resolution, the ASPEX has the advantage of fast
metallographic sample, a 20 mm billet slice was divided scanning and automatic feature analysis resulting in a
into 49 samples, each measuring 20 mm by 20 mm, as large number of particles in a sample being analyzed in
illustrated in Figure 2(b). several hours. A sample measuring 20 9 20 mm2 was
selected for analysis on each metallographic specimen
and the electron beam scanned the random area on the
B. Analysis Methods 20 9 20 mm2 sample until a 9.8 mm2 scanned area was
The analysis of oxygen was performed using a Leco analyzed. The minimum particle size was set at 0.6 lm,
Oxygen Analyzer in which the sample was melted inside which means that the ASPEX 1020 was sensitive to only
a graphite crucible and the product gas quantified by a inclusions larger than 0.6 lm. The types of inclusions
detector and converted to the total oxygen content. The were categorized according to the weight percentage of
elements detected in them. The rule file is shown in indicates the morphology of inclusions by ASPEX
Table II. In order to observe the three-dimensional (Figure 3). The typical inclusions in the steel billets are
morphologies of inclusions, typical morphologies of alumina-based clusters, alumina magnesia (Al2O3-MgO)
inclusions were revealed using partial acid extraction. A spinel single or cluster inclusions, silicon oxide (SiO2)
36 pct HCl solution was used as the solvent. Morphol- bearing spherical inclusions, separate sulfide-based
ogies and compositions of inclusions on a steel sample inclusions, and irregularly shaped slag inclusions con-
(32 9 25 9 15 mm3) at different extraction times were taining calcium oxide (CaO), potassium oxide (K2O),
compared. and sodium oxide (Na2O). Alumina (Al2O3) inclusions
mainly stem from deoxidation by aluminum or reoxi-
dation of the residual aluminum in the steel. Inclusions
III. MORPHOLOGY AND COMPOSITION high in magnesium oxide are a result of the reaction
OF INCLUSIONS between molten steel and magnesium refractory, espe-
cially the tundish lining refractory. Inclusions with
Figure 3 shows the typical morphology and compo- sodium (Na) and potassium (K) are from the entrain-
sition of inclusions in the billet sample, which clearly ment of the mold slag. Sulfide inclusions mainly
Fig. 3—Inclusion morphology and composition (in mass pct) observed by SEM (polished sample).
Fig. 4—Inclusion morphology and composition (atomic pct) observed by SEM (etched by acid).
O 69.1%
(a) Al 28.0%
Ca 2.9%
O 67.2%
Mg 6.0
(b)
Al 25.9%
Ca 0.9%
O 60.0%
(c) Al 39.1%
Ca 0.9%
O 58.5%
(d) Al 26.2%
Ca 15.3%
O 68.8%
Al 8.7%
(e)
Si 15.0%
Mn 7.4%
Fig. 5—Typical inclusions after different time acid extractions (the numerical value in the top right corner is the acid extraction acid time).
Fig. 7—Clogging materials (mainly Al2O3-CaO-MgO inclusions) at the submerged entry nozzle.
precipitate during cooling and solidification of the steel. analytical time and storage space for thousands of
The optical resolution from ASPEX was set for provid- counted inclusions.
ing sufficient information to determine the diameter, The morphology and composition of typical inclu-
area, and perimeter of inclusions with reasonable sions etched by acid were detected using SEM–EDS
large inclusions are particularly harmful to the mechan- B. Spatial Distribution of Inclusions
ical properties, acting as stress concentrators or casing The distribution of inclusions with various composi-
surface cracking. Figure 10 indicates that there were more tions in the billet had special significance and it provided
>20 lm inclusions measured on the cross section of the information about the distribution of alumina-based
billet during ladle change (S2) than that at the steady state inclusions stemming from deoxidation,[18,36] reoxidation,[37]
(S1) due to the fact that more slag was entrained and more entraining refining slag,[38] or refractory materials.[39,40]
air was absorbed at the unsteady state than steady state.
Thickness (mm)
2.0 2.0
90 90 2.0
Thickness (mm)
105 2.0 105 2.5 2.0
2.5 1.5 1.5 1.0
2.0
90 3.0 90 2.0 3.0
75 4.0 75 2.5 4.0 5.0 3.5 1.0
2.0 4.0
60 5.0 60 1.0 2.5 5.0
1.5 2.0 3.0 2.5 1.5 1.5 4.5 4.0
45 45 2.5
3.0 3.5
30 1.5 30 3.0
1.5 1.5 0.5 2.5 3.0
15 15
1.0 2.5
2.5
0 0
0 15 30 45 60 75 90 105 120 135 150 0 15 30 45 60 75 90 105 120 135 150
Outer Radius (mm) Outer Radius (mm)
(a) Steady state (S1) (b) Ladle change (S2)
Fig. 12—Distribution of oxide inclusions on cross section of the billet.
Thickness (mm)
of 5 lm oxides on the cross section of the billet under As is well known, the total oxygen can reflect the
steady state (S1) is shown in Figure 16. At the initial level of inclusions and cleanliness of billet. The total
solidification, the distance between the dendrite arms oxygen results directly detected by the Leco oxygen
can only provide space for smaller inclusions, whereas analyzer are shown in Figure 17. Under steady-state
the approaching larger inclusions might be pushed casting (S1), the total oxygen concentrated at the
away. As the dendrites grow, the dendrite spacing has center of the billet and the average total oxygen was
the capacity to entrap much larger inclusions. 10.3 ppm. During the ladle change period, the total
Thickness (mm)
Thickness (mm)
105 8 105 8
14 2 2 10 4
90 18 10
12 90 6 12
2
6 14 14
75 16 75 2 16
18 8 18
60 2 60 2 18
45 2 12
45 6 16
30 2 30 12 8 6 10 16
2
15 15 10
4
0 0
0 15 30 45 60 75 90 105 120 135 150 0 15 30 45 60 75 90 105 120 135 150
Outer Radius (mm) Outer Radius (mm)
(a) Steady state (S1) (b) Ladle change (S2)
Thickness (mm)
2.0 3
90 2.5 90 4
6
3.0 75 3 5
75 1.5 2.0 1.5
2.0 4 6
60 4.0 60
1 1 2 4
2.5 2.0 1.5 2.5 2 3
45 3.0 45
30 2.5 30 2
2.5 2.0 1.5 1.5 1
15 15 1
1.0
0 0
0 15 30 45 60 75 90 105 120 135 150 0 15 30 45 60 75 90 105 120 135 150
Outer Radius (mm) Outer Radius (mm)
(a) 1 µm oxides (b) 5 µm oxides
Inner Radius (mm)
150 Num%
4 2
135 1
0
120 4 1
2
Thickness (mm)
105 2 6 3
90
5 4
75 5
6
60 4
3 5
45
1
30 3
15 3
2 1
0
0 15 30 45 60 75 90 105 120 135 150
Outer Radius (mm)
(c) >5 µm oxides
Fig. 15—Distribution of different size oxide inclusions on the measured cross section of the billet under steady state (S1).
Thickness (mm)
12 7 18
14 14
90 12 11 90
13 17 14 17 15 16 17
75 75 17 15
17 20 16 16 20
60 15
16 60
18
10 10 14 16 15
45 45 16 16
15
30 11
30 16
14
18 17
16 17 16
15 15
15 15
0 0
0 15 30 45 60 75 90 105 120 135 150 0 15 30 45 60 75 90 105 120 135 150
Outer Radius (mm) Outer Radius (mm)
(a) Steady state (S1) (b) Ladle change (S2)