ISC Research Symposium

Spring 2010

Effect of Argon Stirring on

Inclusion Flotation Using a
Porous Plug

Advisor:
Dr. K. Peaslee

Andrew OLoughlin

April 12, 2010

Abstract:
This report documents the use of argon stirring with a porous plug in 1000lb ladles to improve the
flotation of inclusions before casting. The effect of the rate of stirring was investigated to determine the
effect on heat los in the ladle (energy considerations), steel cleanliness and gas content of nitrogen and
oxygen. The trial did not show improvements in cast properties over the standard ladle practice, but in
fact the application reduced steel cleanliness. The effectiveness of the method was limited by the ability
to stir the melt without breaking the protective slag surface layer.

Introduction:
Inclusions predominately entrapped oxides and sulfides in steel that serve as the primary sites for
void nucleation and growth of crack propagation. To improve the mechanical properties of steel, ladle
treatments are applied to improve inclusion flotation through deoxidization reactions (Ca treatment) or
stirring the melt with inert gas. Argon stirring with a porous plug is a common practice in industrial
continuous casting operations and larger foundry ladle operations. Stirring with argon promotes the
flotation of inclusions and dissolved gases (H, O and N), and aid in the homogenization of the melt
chemistry and temperature[1]. The use of porous plugs in large ladles (greater than 40 tons) offer several
advantages over lance stirring. These include: better stirring at the bottom of the ladle, the protective slag
layer at the surface of the melt is not broken (for a nonviolent stir rates), and more efficient operational
controls [2]. In a previous study conducted by Vintee Singh, the practice of argon lance stirring and Ca
wire treatment were investigated in 1000lb ladles. The trial showed a slight improvement in inclusion
flotation using the lance stirring, but the Ca wire treatment provided a significant improvement in steel
cleanliness [3].

Experimental Procedure:
The Ar stir rate was studied for seven ladles of medium carbon steel (Table I). For each ladle,
steel chemical samples were collected before stirring, after stirring, part way through the pour and the
mold. The three ladle samples were collected using submerged chemistry samplers. Keel bar molds were
cast for each to provide material for Charpy impact tests. The temperature of the melt was monitored at
each process step to monitor the rate of heat loss in the melt. The Ar flow rate was controlled to provide
three different levels of stirring: a short violent stir (2.9 CFM for 2 min), a gentile stir (1.0 CFM for 4 and
4.5 min) and a medium stir (1.9 CFM for 1, 2, and twice at 3 min).
Table I: Average Chemistry of the Steel Castings.
C
0.20 to
0.25

Mn
0.45 to
0.51

P
0.010 to
0.012

S
0.018 to
0.019

Si
0.43 to
0.47

Cu
0.075 to
0.067

Ni
0.104 to
0.048

Mo
0.031 to
0.027

Cr
0.243 to
0.125

V
0.008 to
0.005

Al
0.107 to
0.08

Ti
0.052 to
0.041

Fe
Bal.

The oxygen and nitrogen gas content was measured using a Leco TC-500. To ensure accurate values,
three 0.7 to 1.0g steel sections were tested per sample. To measures the oxygen and nitrogen, the machine
melts the steel coupons in an electrode impulse furnace and runs solid state infrared and thermal
conductivity measurements on the molten pool. The steel cleanliness was evaluated using an ASPEX
analytical SEM particle analyzer to quantify the inclusion content. Over 1000 inclusions per sample were
dimensionally analyzed and compositionally analyzed using EDX 1000. To compare the inclusion
analysis to the previous Ca-Wire injection study, the same inclusion classification rules were used
(according to EDX composition). The keel bars were normalized at 1650oF for 1.5 hrs and air cooled.
Three V-Notch Charpy impact bars were machined for each condition and were tested at -40oF.

Results and Discussion:

A complete overview of the Ar stir trials is provided in Table II. The change in inclusion and gas
content throughout the processing steps contains significant scatter, but there is a steady trend of
increasing the fraction of inclusion coverage with processing steps. This is contrary to the previous study
conducted by Vintee Singh, where the inclusion content declined with ladle hold time and Ar Stirring [3].
Table II: Overview of the porous plug Ar-stir trial ladle treatments.
Heat and Ladle Number

34832-2

34901-1

4.5

1.9

1.9

1.9

1.9

2.9

3046

2962

2967

2959

2985

2955

2955

2976

Inclusion Count (#/mm )

748

792

916

1311

980

1311

1155

1030.4

Inclusion Coverage (m2/mm2)

845

1087

1144

1485

1861

1325

1226

1281.9

Oxygen (ppm)

152

131

121

135

127

103

200

138.4

237.6

199.9

208.8

216

215

221.8

227

218

2933

2858

2906

2925

2868

2855

2904

2893

Inclusion Count (#/mm )

737

696

696

833

981

1088

884

845

Inclusion Coverage (m2/mm2)

1192

1637

1256

2085

1503

2295

2320

1755.4

Oxygen (ppm)

121

97.6

88.3

155

112

88.4

77.1

105.6

223.8

177.3

203.2

184.9

200

223

186.6

199.8

305

264

356

473

293

484

326

357.3

4110

10693

5112

2948

10109

3256

5423

5950.1

Stir Time (min.)

Stir Rate (CFM)
o

Temperature ( F)
2

Before Stir Nitrogen (ppm)

o

Temperature ( F)
2

After Stir

Nitrogen (ppm)
2

Inclusion Count (#/mm )

2

Inclusion Coverage (m /mm )

34901-2 34901-3 34902-1 34902-2 34902-3 Average

Oxygen (ppm)

80.1

75.5

81.1

85

88

80.1

69.3

79.9

Nitrogen (ppm)

190.1

157.1

177.4

168

183.3

190.1

187.3

179

Final Casting Charpy Impact Energy (Ft-lbs) 6.3 0.7 8.2 0.4 9.2 1.6 6.9 0.4 5.6 1.1 6.5 0.3 6.1 1.1 7.0 1.4

Appendix A provides a comparison of the inclusion content, O and N levels and the impact
toughness measurements from the keel bar mold samples for all of the porous plug trails and the inclusion
and toughness measurements from the previous trial (Ar stirring with a lance and Ca-wire injection). The
primary difference between the inclusion content in the two studies can be attributed to elevated levels of

MnS and TiO detected in the porous plug trials (Figure 1 b and Figure 2). Two measurements of the
inclusion content were reported. The inclusion count (number of inclusions per mm2) and the inclusion
coverage (area fraction of inclusions over the area of metal scanned). The inclusion coverage is a better
indicator of steel cleanliness, because is accounts for the size of inclusions. The inclusion content and
inclusion coverage data for the porous plug showed significant scatter and did not follow the expected
trend of decreasing fraction area covered with increasing stir time (Figure 1 a & b). The gas content in
the final castings was stable and did not show any trend with increasing stir time or stir rate (Figure 1c).
The oxygen values were low (~70 to 90 ppm) and did not vary with differences in oxides inclusions. In
comparison, the nitrogen values were large (160-190 ppm), but if is not uncommon for foundries to
contain large nitrogen content. When compared to the previous trial data shown in Figure 2, the fraction
of area covered by inclusions in the porous plug samples was substantially greater that the untreated
standard practice trial (0.01 to 0.003 compared to 0.001 area of inclusions over the surface area
scanned). The Charpy impact testing observed very low energy absorbed values ranging from 5 to 9 ft-lbs
(Figure 3a). This was comparable to the lower limit of mechanical properties observed in the Ca-wire trial
(Figure 3b).
Ar stirring with the porous plug was not an appropriate ladle treatment method to improve the
mechanical properties of the 1000lb ladle castings. The negative impact of Ar stirring on inclusion
content indicates the protective slag layer was disrupted even at low stir rates. The 1000 pound ladles
are at a disadvantage to larger ladles (greater than 40 ton), because the heat loss at the slag line is
substantially larger due to surface area to molten metal ratio. Therefore for smaller ladles, the benefits of
improved inclusion flotation are negated by unstable slag lane.

Conclusions:
Argon stirring with a porous plug in 1000lb steel ladles did not improve inclusion flotation, but
degraded steel cleanliness by introducing large levels of TiO2 and MnS. This was validated by
quantitative inclusion measurements and Charpy impact testing.

References:
[1]
[2]
[3]

Lalhua Wang, Hae-Geon Lee, Peter Hayes, A New Approach to Molten Steel Refining
Using Fine Gas Bubbles, ISIJ International Vol 36 (1996), No 1 pp 17-24.
Alan Cramb, The Making Shaping and Treating of Steel, Casting Volume, 11th Edition,
AISE Steel Foundation, Pittsburgh, 2003.
Vintee Singh, Inclusion Modification in Steel Castings using Automated Inclusion Analysis,
M.S. Thesis, University of Missouri Science and Technology, Rolla, 2009.

Number of Inclusions (No. / mm )

Appendix A Comparison of Cast Keel blocks from all of the Ladle Trials
Other

600

TiO2

500

CaO

400

Al2O3
MnO

300

MnSiO3
CaS

200

MnS

100
0
34902-2
34832-2
34902-1
34901-1
34901-2
34901-3
34902-3
Ar 4.5 min. Ar 4 min. Ar 3 min. Ar 3 min. Ar 2 min. Ar 1 min. Ar 2 min.
(1.0 CFM) (1.0 CFM) (1.9 CFM) (1.9 CFM) (1.9 CFM) (1.9 CFM) (2.9 CFM)

Fraction of Area Covered by Inclusions

a. Number of inclusions per mm2 in the cast keel bar for the porous plug Ar-stir trials.
Other
0.01

TiO2
CaO

0.008

Al2O3

0.006

MnO
MnSiO3

0.004

CaS
MnS

0.002
0
34902-2
Ar 4.5 min.
(1.0 CFM)

34832-2
Ar 4 min.
(1.0 CFM)

34902-1
Ar 3 min.
(1.9 CFM)

34901-1
Ar 3 min.
(1.9 CFM)

34901-2
Ar 2 min.
(1.9 CFM)

34901-3
Ar 1 min.
(1.9 CFM)

34902-3
Ar 2 min.
(2.9 CFM)

Amount of Oxygen and Nitrogen (ppm) .

b. Fraction of area covered by inclusions in the cast keel bar for the porous plug Ar-stir trials.
Oxygen

250

Nitrogen
200
150
100
50
0
34902-2
Ar 4.5 min.
(1.0 CFM)

34832-2
Ar 4 min.
(1.0 CFM)

34902-1
Ar 3 min.
(1.9 CFM)

34901-1
Ar 3 min.
(1.9 CFM)

34901-2
Ar 2 min.
(1.9 CFM)

34901-3
Ar 1 min.
(1.9 CFM)

b. The oxygen and nitrogen content in the cast keel bar for the porous plug Ar-stir trials.

Figure 1: The inclusion content in the cast keel bars for all of the Ar-stir trails.

34902-3
Ar 2 min.
(2.9 CFM)

Fraction of area covered by inclusions

Others

0.0018

TiO2

0.0016

CA

0.0014

Al2O3

0.0012

MnO
MnSiO3

0.001

CaS

0.0008

MnS

0.0006
0.0004
0.0002
0
0.00 % Ca
0.00 ft/min
No Stir

Ladle Stir 0.024% Ca 0.028% Ca 0.032% Ca 0.043% Ca 0.043% Ca 0.05% Ca 0.06% Ca

12.5 ft/min 12.5 ft/min 12.5 ft/min 12.5 ft/min 12.5 ft/min 12.5 ft/min 20 ft/min
No Stir
No Stir
No Stir
No Stir
Ladle Stir
No Stir
No Stir

Charpy Impact Energy Absorbed (ft-lbs)

Figure 2: Fraction of area covered by inclusions in the cast mold for all trials of the Ca-wire injection
study.
Note: The first two trials (an untreated ladle and in ladle Ar lance stir) provide a good perspective to
the porous plug Ar-stir trials.
18
16
14
12
10
8
6
4
2
0
34902-2
Ar 4.5 min.
(1.0 CFM)

34832-2
Ar 4 min.
(1.0 CFM)

34902-1
Ar 3 min.
(1.9 CFM)

34901-1
Ar 3 min.
(1.9 CFM)

34901-2
Ar 2 min.
(1.9 CFM)

34901-3
Ar 1 min.
(1.9 CFM)

34902-3
Ar 2 min.
(2.9 CFM)

Charpy Impact Energy Absorbed (ft-lbs)

a. Charpy impact energy absorbed for all ladle treatments conducted in the porous plug Ar-stir trials.
18
16
14
12
10
8
6
4
2
0
0.00 % Ca
0.00 ft/min
No Stir

Ladle Stir 0.024% Ca 0.028% Ca 0.032% Ca 0.043% Ca 0.043% Ca 0.05% Ca 0.06% Ca

12.5 ft/min 12.5 ft/min 12.5 ft/min 12.5 ft/min 12.5 ft/min 12.5 ft/min 20 ft/min
No Stir
No Stir
No Stir
No Stir
Ladle Stir
No Stir
No Stir

b. Charpy impact energy absorbed for all ladle treatments conducted in the Ca-Wire injection trials.
Note: The dashed lines are the maximum and minimum Charpy impact values observed in the porous plug
trial and the solid line is the average Charpy impact value.

Figure 3: Charpy impact energy measurements for normalized keel bars samples.