Novel Fluxing Agents for Ladle Slags to Improve

Refractory Life Time and Steel Quality

C. Wöhrmeyer, R. Jolly, C. Brüggmann

Flux melting interval
To improve the life time of ladle slag zone bricks the impact of nov-
el synthetic pre-reacted Calcium Magnesium Aluminate Fluxes (OP- Calcium Aluminate Flux (LDSF ®RG)

TIMET™ RG and OPTIMET™ HM) has been studied. They bring the
MgO content in the slag immediately after tapping steel from con- 1300°C 1320°C 1325°C 1340°C

verter or electric arc furnace into the ladle throughout the whole slag Calcium Magnesium Aluminate Flux (OPTIMET ™RG)

mass close to the saturation concentration. That minimises the chem-

ical dissolution of MgO from Magnesia-Carbon or Dolomag-Carbon 1320°C 1340°C 1345°C 1360°C

bricks. Longer refractory live time is the positive effect. OPTIMET™

forms very rapidly a homogeneous and liquid slag with a high ca- Fig. 1 Melting behaviour of Calcium
Aluminate flux and Calcium Magnesium
pacity to absorb sulphur and oxide inclusions from the steel bath, a Aluminate flux (test method as described
prerequisite for efficient clean steel production. This new fluxing in DIN 51730, heating rate 10K/min)
practice with Calcium Magnesium Aluminate helps to reduce the spe-
cific costs per tonne of steel. The efficiency of high quality steel pro- as consequence of the formation of a very
low viscose slag, synthetic calcium alumi-
duction can be increased and production capacities be optimised.
nate fluxes (LDSF® RG) have become part of
These novel fluxing agents support the efforts to reduce the CO2- modern steelworks practice especially where
emissions per ton of produced steel. clean steel production is required [8, 9]. Cal-
cium aluminate fluxes combine the advan-
tage of creating quickly a homogeneous and
1 Indroduction slag as early as possible and to reduce the sufficient liquid slag with the chemical capa-
Refractory linings in steel ladles are exposed driving force for the MgO-dissolution from city to absorb a large variety of non-metallic
to steel, slag, and air at temperatures up to refractories. In some cases steelworks add
1650 °C. Especially the contact zone be- for example doloma directly to the slag as an
tween the refractory material and the metal- external source for MgO [5]. Christoph Wöhrmeyer, Remi Jolly
lurgical slag have been studied by many au- But fusion and homogenisation of coarse Kerneos Aluminate Technologies
thors with the objective to improve the re- MgO or (Ca, Mg)O grains takes time while 92521 Neuilly-sur-Seine, France
fractory lining [1–3]. Different degradation dissolution of the fine grains from the matrix
phenomena occur in this zone which are of the bricks is already in progress. Addition Christian Brüggmann*
combinations of thermo-chemical and ther- of powders of magnesia and doloma to the German Refractory Research Association
mo-physical processes [4, 5]. The thermo- slag should be avoided to prevent dust for- (FGF e.V.)
chemical reactions are seen as a major de- mation and introduction of humidity into the 53113 Bonn, Germany
gradation cause since the slag compositions system since both doloma and magnesia
are typically under-saturated in MgO. That powders tend to hydrate in humid air [7]. Corresponding author: C. Wöhrmeyer
creates a chemical gradient between the E-mail: christoph.wohrmeyer@kerneos.com
MgO-containing bricks and the slag. As con- 2 Materials and methods
sequence dissolution reactions occur [6]. 2.1 OPTIMET™ RG and Keywords: synthetic slag, calcium alumi-
This study is designed to improve refractory OPTIMET™ HM – the new nates, calcium magnesium aluminates, calci-
life time and thus reduce operational costs synthetic fluxing materials um fluoride, refractory wear, secondary steel
by modifying the slag with the novel fluxing Traditionally, CaF2 was used to create a fluid ladle
materials OPTIMET™ RG and OPTIMET™ steelworks slag in mixes for example with
HM. They are based on pre-reacted synthet- bauxite and lime. But due to the environ- *) Present address: ThyssenKrupp Nirosta
ic calcium magnesium aluminates. The ob- mental problematic with fluorine and fur- GmbH, Krefeld, Germany
jective is to increase the MgO-content in the thermore due to the strong corrosion effect

refractories WORLDFORUM 3 (2011) [3] 81

Tab. 1 Chemistry of synthetic calcium magnesium aluminate flux (OPTIMET™) and advantage of having an increased MgO-lev-
calcium aluminate flux (LDSF® RG) el in the slag right from the beginning com-
OPTIMET™ HM OPTIMET™ RG LDSF® RG pared to a normal calcium aluminate or a
CaF2 practise.
Pre-reacted Pre-reacted Pre-reacted
CaO 32,9 37 50,5 2.2 Thermo-chemical calculations
MgO 21,3 12,5 0,6 After tapping steel into the ladle and having
Al2O3 40,9 43 41,5 added traditional fluxing materials to it the
SiO2 3,6 3,6 3,4
initial slag composition at the beginning of
the ladle treatment contains often between
FeO 1,7 1,7 1,7
3 and 7 % MgO. The MgO-saturation con-
TiO2 2,2 2,2 2,3 centration of model slag compositions as
CaF2 0 0 0 shown in Tab. 2 have been calculated using
H2O < 0,15 < 0,15 < 0,15 the FactSage© software [11]. The MgO-satu-
ration concentration is dependent on the
CO2 < 0,1 < 0,1 < 0,1
slag basicity, temperature, FeO- and CaF2-
Total 100 100 100
content. For the range of the considered
(CaO + MgO) / Al2O3 1,3 1,2 1,2 compositions (Tab. 2) with basicity B be-
tween 0,7 and 1,5 with
impurities from the steel bath and support MET™ HM of about 21 %. Both are free of
as well the de-sulphurization process. The impurities like fluorine, carbon, and humidi- B = CaO / (Al2O3 + SiO2) (1)
rapid modification of the Al2O3 / SiO2 ratio by ty. The increased MgO content compared to
pre-reacted calcium aluminate phases plays LDSF® RG has no negative impact on the and temperatures T between 1500 and
an essential role in this regard. metallurgical efficiency, for example the de- 1620 °C the following equation (2) derived
The new synthetic calcium magnesium alu- sulphurization effect [10]. which describes the MgO-saturation of the
minate fluxes OPTIMET™ RG and OPTI- The melting behaviour of OPTIMET™ RG is slag:
MET™ HM contain MgO in microcrystalline almost equal to LDSF® RG as can be seen in
phases and can be added to the slag in form Fig. 1. At 1345 °C it is already almost liquid (% MgO)sat = 8,2 / B + 0,06 (%FeO) +
of dust-free aggregates in the same way as and starts to flow at 1360 °C. OPTIMET™ 0,2 (%CaF2) + 0,019 (T –1550) (2)
classical calcium aluminate fluxes. HM has the same melting behaviour. It takes
As can be seen in Tab. 1 OPTIMET™ RG has only 1 minu at 1600 °C to create a homo- The results of this equation are in good
a MgO-content of about 12 % and OPTI- geneous liquid top slag (Fig. 2). This has the agreement with experimental results from
[6]. As can be seen from the equation (2) the
levels of basicity and as well the temperature
have a strong impact on the MgO-saturation
concentration followed by the amount of
CaF2 present in the slag. It shows that all
considered initial slag compositions with the
exception of No. 5 are under-saturated with
MgO and have the potential to dissolve the
lacking MgO-content from MgO-C or Dolo-
mag-C bricks. With the OPTIMET™ fluxes
the gap between the initial MgO-concentra-
tion and the MgO-saturation will be reduced
very fast and homogeneously throughout
the whole slag mass. Especially the rapidity
and homogeneity of introduction of MgO
into the slag is much more difficult to
achieve by separate MgO-additions in form
of magnesia or doloma. In order to verify this
and to estimate the impact of kinetics prac-
tical experiments have been set up.

2.3 Test methods

Fig. 2 Fluxing behaviour of LDSF® RG (slag C; left) and OPTIMET™ RG (slag A-2; right) To simulate the conditions in the steel
at 1600 °C ladle slag line a laboratory induction furnace

82 refractories WORLDFORUM 3 (2011) [3]

Tab. 2 Slag compositions that have been used for thermodynamic simulations of MgO- in Al-killed steel production at the beginning
saturation (FS = results from FactSage© simulations; E2 = results from equation 2) of the steel treatment in the ladle have been
1 2 3 4 5 targeted to compare the different fluxing
CaO 44,0 44,9 41,6 35,0 50,0 practises.
Slag A-1 and A-2 use an addition of 20 %
MgO 6,0 6,1 5,7 7,0 6,8
OPTIMET™ HM respectively 20 % OPTI-
Al2O3 34,0 34,7 32,2 39,5 25,0
MET™ RG to the total slag mass and slag C
SiO2 9,0 9,2 8,5 10,4 10,2
the same amount of LDSF® RG flux.
FeO 7,0 5,0 12,0 8,1 8,0 Slag B has also been fluxed with LDSF® RG
CaF2 0,0 0,0 0,0 0,0 0,0 but 2 % of sintered magnesia in the grain
Basicity B 1,02 1,02 1,02 0,70 1,42 size of 3 – 6 mm have been added supple-
(MgO)sat 1550 °C (FS) 8,6 8,5 8,9 12,0 5,8 mentary.
(MgO)sat 1550 °C (E2) 8,4 8,3 8,7 12,2 6,3 In case of Slag D 3,5 % fluorspar has been
Liquidus [°C] (FS) 1395 1406 1366 1372 1614 used as fluxing agent. In preliminary trials
with a holding time of 60 min it was found
6 7 8 9 10 that the MgO-concentration reaches almost
its saturation level after 30 min already so
CaO 38,7 46,9 42,7 40,5 37,8
that it was preferred to run cycles of 30 min
MgO 5,3 6,4 5,8 5,5 5,2
only to achieve a maximum of corrosion ef-
Al2O3 42,0 36,2 33,0 31,3 29,2
fect during a 6 h trial.
SiO2 7,9 3,0 8,7 8,3 7,7
Every 30 min the total slag mass has been
FeO 6,2 7,5 6,8 6,4 12,0 removed and replaced by fresh slag and flux.
CaF2 0,0 0,0 3,0 8,0 8,0 A total holding time of 6 h, thus 12 slag cy-
Basicity B 0,78 1,20 1,02 1,02 1,02 cles (heats) have been applied with the
(MgO)sat 1550 °C (FS) 11,0 7,3 9,2 9,9 10,1 same slag practice. During this time the steel
(MgO)sat 1550 °C (E2) 11,0 7,3 9,0 10,0 10,3 remains inside the vessel at 1600 °C. Only
Liquidus [°C] (FS) 1373 1495 1339 1322 1347 the slag has been replaced after each heat.
After the 6 h-trial the 8 MgO-C segments
have been cut and the corrosion depth was
as described in [12] has been chosen as furnace. The furnace is charged with blocks measured.
test vessel in which MgO-C bricks or of 15 kg of steel (with 0,1 % C, 2,65 % Si, Since the doloma is quite sensitive to hu-
(Ca, Mg)O-C bricks build the side wall. 1,65 % Mn, 0,014 % P, 0,0006 % S and midity special care had to be taken for the
The employed MgO-C brick material con- 0,035 % Al) which are heated up by induc- sample preparation and it was decided to
tains 12 % carbon. The oxide components tion under Ar / H2 atmosphere to the test dry-cut rectangular Dolomag-C segments
are 97 % MgO, 1,7 % CaO, 0,6 % SiO2, temperature of 1600 °C. Then 480 g of a from the bricks. Here only four segments
0,5 % Fe2O3 and 0,2 % Al2O3. The density is slag (579 g in case of slag D) is formed on build the wall in the induction furnace. The
3,01 g/cm3 and open porosity 4,0 %. Seg- top of the liquid steel to which then 120 g of furnace has been charged with 4 kg of steel
ments with trapezoidal cross section have the fluxing materials (21 g in case of CaF2 only and a total of 400 g of slag including
been cut from this brick material. Eight for slag D) as grains of 3 – 6 mm are added the amount of fluxing material (7 % for
of these segments build the side wall of the (Tab. 3). Slag compositions as can be found LDSF® RG and OPTIMET™, 3,5 % in case of

Tab. 3 Slag chemistry of the liquid part of the slag 1 min after flux addition [mass-%]

Slag A-1 Slag A-2 Slag B Slag C Slag D

Fluxing with OPTIMET™ HM OPTIMET™ RG LDSF®RG + MgO LDSF® RG CaF2
Flux in slag 20 % 20 % 20 % LDSF 2 % MgO 20 % 3,5 %
CaO 53,5 54,1 56,8 57,4 53,3
MgO 7,0 5,8 4,1 3,9 3,8
Al2O3 27,2 27,6 27,2 26,9 25,9
SiO2 9,2 9,4 9,0 9,2 9,9
FeO 3,1 3,1 2,9 2,7 3,4
(CaF2) 0 0 0 0 (3,5)
Basicity B 1,47 1,46 1,57 1,59 1,49
MgOliq+sol, after 1min 8,1 6,3 6,3 3,9 3,8
MgOsat 6,8 6,8 6,3 6,3 7,4

refractories WORLDFORUM 3 (2011) [3] 83

 rate of 20 % in both cases. Almost all MgO
is already after 1 min inside the liquid phase
while in case of slag B practically non of the
added MgO has been transferred yet into
liquid at this stage. By measuring the aver-
age of the lost diameter for the 8 MgO-C
segments employed in the furnace wall of
one test run it becomes obvious that CaF2
creates the strongest corrosion (Figs. 3, 4).
LDSF® RG represents already an improve-
ment compared to CaF2. Significantly better
is the use of OPTIMET™ RG and OPTI-
MET™ HM which causes by far the lowest
corrosion. In case of the slag practice with
OPTIMET™ RG a high initial MgO level
could be achieved (Fig. 5) and consequently
only a small increase of MgO has been ob-
served after 30 min which translates into the
Fig. 3 MgO-C-brick corrosion profile as function of slag fluxing practise low corrosion rate.
With OPTIMET™ HM the initial MgO-con-
tent in the slag reaches already at this very
1,2
early moment the MgO-saturation limit
1,1 (Fig. 6) which explains the very low corro-
sion rate when OPTIMET™ HM is employed
1
Corrosion rate [mm / h]

into the slag. The biggest increase in MgO

0,0 was observed with the CaF2 practice which
explains the strong corrosion in that case.
0,8
On the other hand with LDSF® RG a similar
0,7 MgO dissolution but a lower corrosion rate
0,6
was observed.
Here it has to be mentioned that the corro-
0,5 sion profile in case of CaF2 is different due to
0,4 the low slag viscosity which more strongly
OPTIMETTM HM OPTIMETTM RG LDSF® RG (20 %) LDSF® RG (20 %) CaF2 (3,5 %) attacks the bond of the MgO-C brick (Fig. 3).
(20 %) (20 %) + MgO (2 %)
As consequence MgO grains from the brick
Fig. 4 MgO-C-brick corrosion rate as function of slag fluxing practice can more easily be removed from the brick
structure by mechanical movements of the
CaF2). The steel is containing 0,03 % C, Semi-quantitative XRF-analyses have been slag [8]. These MgO grains can float as solid
0,03 % Si, 0,3 % Mn, 0,02 % P, 0,02 % S conducted on pressed powder samples. particles inside the slag when slag is already
and 0,005 % Al. saturated with MgO. During slag sampling
The tests have been conducted here as well 3 Results with a steel rode it is unlikely that a solid
at 1600 °C and Ar / H2 atmosphere. Every 3.1 Magnesia-C brick in contact grain will be taken together with the liquid
30 min the slag has been replaced by fresh with Al-killed ladle slag part of the slag. This explains why the meas-
slag. The total slag contact time was 3 h Some of the different slag practices that ured MgO concentration after 30 min is in
(6 cycles). have been tested are shown in Tab. 3 with all cases close to 7 %, the MgO saturation
For each slag practice the furnace has been their initial composition (liquid part of the limit.
newly equipped with fresh segments of the slag after 1 min of flux addition). The values Although OPTIMET™ RG and LDSF®RG +
same MgO-C or (Mg, Ca)O-C material and are average analyses from the first 2 (in MgO bring theoretically the same total
fresh steel of the same quality has been some cases 3) heats. The theoretical MgO- amount of MgO into the slags A-2 and B, the
charged. saturation has been calculated from formula faster dissolution of MgO in case of OPTI-
During all tests slag samples have been tak- (2) for 1600 °C. MET™ creates an advantage over an exter-
en with a steel rod to follow the evolution of As can be seen in Fig. 2 OPTIMET™ flux cre- nal MgO addition. Due to the slow dissolu-
the chemical composition of the slag as a re- ates rapidly a liquid slag (e.g. slag A-2) tion rate of the added MgO grains corrosion
sult of the refractory corrosion. During the which increases the amount of MgO in the is consequently stronger than in case of OP-
short slag sampling process, the slag surface liquid phase almost instantaneously by 2 % TIMET™. It was discovered by [1] that a
is exposed to normal air. compared to LDSF RG (slag C) at an addition dense MgO grain of 20 mm in diameter im-

84 refractories WORLDFORUM 3 (2011) [3]

mersed in different slags is loosing only be- MgO-liq 30 min MgO-liq 1 min
tween 0,6 and 2,2 mm of its diametre in
8
15 min.

OPTIMET™HM (20%)
It has also been tested how a reduced addi-

OPTIMET™RG (20%)
7

LDSF® RG (20%) + MgO (2%)

tion rate of OPTIMET™ behaves. By adding

[%]
only 10 % of OPTIMET™ RG flux thus ap-

(%)

LDSF® RG (20%)
proximately 1 % additional MgO the corro- 6

MgO-liq
MgO-liq

CaF2 (3.5%)
sion was found in the same range as with
slag B with 20 % LDSF® RG + 2 % MgO. This 5
indicates again that the MgO employed in
the OPTIMET™ grains dissolves more rapid- 4
ly in the slag than the externally added
MgO-grains. 3
0,5 0,6 0,7 0,8 0,9 1 1,1 1,2
3.2 Dolomag-C brick in contact Corrosionrate
Corrosion rate [mm/h]
(mm/h)
with Si-killed ladle slag
Fig. 5 Corrosion rate and MgO content in the liquid phase of the slag 1 min and 30 min
Similar positive effects on refractory life time after flux addition
have been found when OPTIMET™ was
used as metallurgical flux for a Si-killed ladle 9
slag in contact with the Dolomag-C bricks
MgO evolution in liquid slag [mass-%]
MgO evolution in liq. slag (wt%)

(Tab. 4). 8 OPTIMET™ HM

While the slag H with CaF2 caused a high
corrosion rate of 1 mm/h it could be reduced 7 OPTIMET ™ RG
by the use of LDSF® RG down to 0,7 mm/h
®
and even to 0,3 mm/h when OPTIMET™ 6 LDSF RG
HM was used. The rapidly soluble MgO in-
side OPTIMET™ HM plays here as well a 5
crucial role. However it has to be mentioned
in case of Dolomag-C bricks that not only 4
the MgO-saturation but also the lime satura-
tion of the slag is crucial to prevent fast dis- 3
solution of the bricks in the slag. 0 5 10 15 20 25 30
Time [min]
Time (min)
4 Conclusion
Fig. 6 Evolution of MgO content in slag in contact with MgO-C bricks as function of flux
OPTIMET™ flux additions to steel-ladle material
slags allow a quick formation of a homoge-
neous liquid metallurgical slag with a high other aspects like mechanical and thermo- software a simplified calculation formula has
initial MgO-content in the liquid phase. The mechanical effects play a role in the degra- been developed which allows very rapidly to
elevated and microcrystalline MgO content dation process of the refractory materials. estimate the real gap between initial MgO
inside OPTIMET™ compared to LDSF® RG Based on simulations with the FactSage© content in the metallurgical slag and the sat-
improves the refractory life of the slag zone
due to the fast gap closing between the ini- Tab. 4 Slag composition before and after fluxing and corrosion rates of Dolomag-C
tial MgO and the saturation concentration in bricks at 1600°C
the slag. This gives an advantage over the Slag E-0 Slag F Slag G Slag H
separate addition of magnesia or doloma as Slag before flux Slag E-0 plus 7 % Slag E-0 plus 7 % Slag E-0 plus
MgO source. Compared to CaF2 practices an addition OPTIMET™ HM LDSF®RG 3,5 % CaF2
improvement of 25 % and compared to a FeO 10,4 9,8 9,8 10,0
LDSF® RG-practice of 15 % has been meas- CaO 56,0 54,4 55,7 54,0
ured in laboratory tests with Magnesia-Car-
Al2O3 9,2 11,4 11,5 9,0
bon bricks when OPTIMET™ RG is used.
OPTIMET™ HM brings further significant SiO2 20,8 19,6 19,6 20,0
improvements of the slag zone durability MgO 3,6 4,8 3,4 3,5
both in case of Magnesia-C- and Dolomag- CaF2 0 0 0 3,5
C bricks. Σ 100 100 100 100
The trials with fluorspar show as well, that
Corrosion rate [mm/h] 0,33 0,68 1,02
further to chemical corrosion effects also

refractories WORLDFORUM 3 (2011) [3] 85

 uration concentration. This helps to select (FGF e.V., Bonn) and DIFK GmbH, Bonn, for (2005) 233–239
the most adapted OPTIMET™ version for conducting the thermodynamic simulations, [6] Reisinger, P.; Preßlinger, H.; Hiebler, H.; Zedni-
each steel ladle configuration and to adjust the practical experiments and for the fruitful cek, K.: MgO-Löslichkeit in Stahlwerksschlak-
the necessary amount of OPTIMET™ flux discussions. ken. BHM 144 (1999) [5] 196–203
addition in an easy and economical way. By [7] Takamiya, Y.: Hydration of crystallized electro-
applying the synthetic OPTIMET™ flux in References fused magnesia in room atmosphere for four
the secondary steel ladle process a signifi- [1] Chen, Y.; Brooks, G.A.; Nightingale, S.A.: Slag years. J. Techn. Ass. Refr. Japan, No. 23-1 (2003)
cant reduction in specific production costs line dissolution of MgO refractory. Canadian 69–70
via the reduction of the specific refractory Metallurgical Quarterly 44 (2005) [3] 323–330 [8] Haratian, M.; Marandian, M.; Aboumahboub,
consumption per ton of steel can be expect- [2] Jansson, S.; Brabie, V.; Bohlin, L.: Corrosion me- A.: The effect of synthetic slag usage on ladle
ed. Results from applications in steel ladles chanism and kinetic behaviour of refractory ma- refractory life. 47th Int. Coll. Refr. Aachen 2004,
have confirmed this positive trend. The met- terials in contact with CaO-Al2O3-MgO-SiO2 pp. 144–147
allurgical efficiency of OPTIMET™ flux en- slags. VII. Int. Conf. on Molten Slags, Fluxes and [9] Olvira, F.C.; Tovar, H.S.; Morelos, J.T.; Mendez,
ables to achieve rapidly the targeted high Salts 2004, pp. 341–347 M.B.: The use of prefused slags in the manufac-
quality steel compositions. This rapidity helps [3] Akkurt, S.; Leigh, H.D.: Corrosion of MgO-C lad- ture of ultra-clean steel in TAMSA. XVIII Simpo-
to safe energy and to optimise capacities of le refractories. Am. Ceram. Soc. Bull. 82 (2003) sio Nacional de Siderurgia, Mexico, 1996
existing steel production processes. The re- [5] 32–40 [10] Lachmund, H.; Xie, Y.; Bruckhaus, R.; Schmitt,
duced specific refractory consumption helps [4] Poirier, J.; Bouchetou, M.L.; Prigent, P.; Berjon- F.J.: Cost effectiveness of DH slag treatment
to safe natural resources. All together OPTI- neau, J.: An overview of refractory corrosion: with optimized metallurgical results. Rev. Metal-
MET™ supports the efforts to reduce specif- observations, mechanisms and thermodynamic lurg. ATS – JSI (2007) 164–165
ic CO2 emissions per ton of produced steel. modeling. Refr. Appl. Trans. 3 (2007) [2] [11] FactSage©: http://www.factsage.com
[5] Blumenfeld, P.; Peruzzi, S.; Puillet, M.: Recent [12] Wöhrmeyer, C.; Jolly, R.; Brüggmann, C.: Novel
Acknowledgement improvements in Arcelor steel ladles through fluxing agent for slags in secondary steel ladles
We would like to thank the teams of the optimization of refractory materials, steel to improve refractory life time and steel quality.
German Refractory Research Association shell and service conditions. Rev. Métallurg. CIT Czech Metallurgical Conference, 2010

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