SME Annual Meeting
Feb. 28-Mar. 03, 2010, Phoenix, AZ
CONTROL OF DISTRIBUTION OF MANGANESE METAL AND SLAG IN IRON NUGGET FORMATION
U. Srivastava, Michigan Tech., Houghton, MI
T. C. Eisele, Michigan Tech., Houghton, MI
ABSTRACT
In the processing of manganiferous ore, it is useful to control
whether the manganese (Mn) goes to the iron product to produce
ferromanganese, or to the slag for extraction as a high Mn product.
This can be done by manipulating the thermodynamic conditions for
manganese oxide(MnO) reduction to control whether it remains as
MnO or converts to metallic Mn. Results are presented showing that
during production of iron nuggets, reduction of manganese oxide
(MnO) can be controlled by changing the furnace temperature and
reductant composition appropriately.
INTRODUCTION
When manganiferous iron ore is used for production of pig iron,
controlling reduction of manganese oxide into metallic manganese has
always been an issue. In industries to reduce manganese oxide in iron
ore, reduction reaction takes place at a very high temperature and at a
very slow rate (Kononov et. el., 2007). From the thermodynamic stand
point higher compounds of manganese oxides (Mn3O4, Mn2O3, and
MnO2) are easily reduced to manganese monoxide (MnO) by carbon
monoxide (CO). Further reduction of MnO by CO is not
thermodynamically feasible, and carbon is needed as reductant to
produce metallic Mn (Berg and Olsen, 1999; Safarian et. el., 2006).
If the reduction process for MnO can be controlled, manganese
can be driven either into pig iron to produce ferromanganese alloy or
into the slag where manganese can be extracted as high manganese
product. Different concentrations of manganese have significant effects
on properties of different grades of steel (International manganese
institute, 2009; Safarian et. el., 2006). Controlling the reduction
process for iron oxide is simpler and easier, compared to manganese.
The reduction process for manganese oxide has been observed at
different temperatures, for different ore compositions and under
different gaseous atmospheres such hydrogen, helium, methane,
argon and etc. (Ostrovski et. el. 2004; Kononov 2008; Kononov et. el.,
2007). However, the effect of different pellets’ composition on
reduction process for manganese has not been yet observed.
The goal of this paper is to study the thermodynamic conditions
and control the reduction process of MnO in iron ore by changing the
pellets’ compositions. Self reducing pellets of different composition
were made from an iron ore sample containing manganese oxide.
These pellets were fired to produce pig iron in nugget form and slag.
Slag was analyzed for the manganese content at different furnace
temperature for different residence times.
Theoretical Discussion
This paper present a study of thermodynamic conditions for MnO
reduction and experiments that were conducted to study the reduction
process of manganese oxide (MnO) that is contained in iron ore. To
reduce present manganese oxide into manganese, thermodynamic
conditions for the reduction of MnO were studied to determine which
conditions could be controlled.
Hypothesis for Thermodynamic Conditions for Manganese Oxide
Reduction
In order to reduce manganese oxide, it is important to understand
the thermodynamics of the reduction reaction. By controlling the
thermodynamics of the reduction reaction, manganese oxide can be
1 Copyright © 2010 by SME
Preprint 10-056
reduced into manganese (Mn). There are two thermodynamic
conditions for manganese oxide reduction that can be controlled:
1) For any reaction, in order to be feasible in forward direction, the
equilibrium constant should be greater than one. When the
equilibrium constant is equal to one, the reaction does not move
in either direction and stays in equilibrium. Based on this theory
manganese oxide reduction by CO as shown in Reaction (1) is
thermodynamically unfavorable due to the presence of CO during
the reverse reaction shown in Reaction (2)
MnO + C Mn + CO (1)
Above, Reaction (1) has very low equilibrium constant, at
-4
temperature 2000K, the equilibrium constant for Reaction (1) is 7 X 10
(Safarian et. el., 2006), which is below one.
MnO + C Mn + CO (2)
To deal with this problem there two things that can be done; a)
the reverse reaction can be minimized by removing CO as quickly as
possible, keeping the its partial pressure low by using pure (99.9%)
carbon instead of coal. Coal contains oxygen and after burning it
produces CO which increases the concentration or partial pressure of
CO; b) by adding some other material to the self reducing pellets to
remove or replace the generated carbon monoxide while the reduction
process when pellets are being fired, so that MnO reduction reaction
does not retard. By changing the pellets’ composition these two
parameters can be controlled. According to Ostrovski and Zhang
(2006), providing the hydrogen atmosphere while firing the pellets
supports the reduction process of manganese oxide. This hydrogen
can also be added to the pellets in the form of some hydrogen
containing chemical instead of providing the atmosphere separately.
2) The other thermodynamic condition that could be controlled is
temperature. Gibbs free energy and Ellingham diagram can be
utilized to calculate the necessary temperature. Gibbs free energy
is a thermodynamic quantity which can be used to determine if a
reaction is spontaneous or not in either direction. Equation (1) is
used for calculating Gibbs free energy.
ΔG = ΔH –TΔS
0
Eq. (1)
Where,
∆G = Gibbs free energy, Joule
0
ΔH = Change in enthalpy, Joule
ΔS = Change in entropy, Joule/K
T = Temperature, K
In order to be feasible and to move in the forward direction for
MnO reduction, the Gibbs free energy of Reaction (1) should be
negative. Gibbs free energy of Reaction (1) can also be calculated by
combining standard Reactions (3) and (4) (Webtool, 2009).
2C + O2 2CO, (3)
∆G = -223,425.6 + (-175.31) T
0
2Mn + O2 2MnO, (4)
 SME Annual Meeting
Feb. 28-Mar. 03, 2010, Phoenix, AZ

∆G = -798,307.2 + (164.85) T
0

The unit of the enthalpy and entropy are in kilojoules (KJ) and
temperature is in Kelvin (K). After subtracting Reaction (4) from (3) we
obtain the desired reaction i.e. Reaction (1) with the Gibbs free energy
equation,
2MnO + 2C 2Mn + 2CO, (5)
∆G = -574,881.6 + (340.16) T
0

Reaction (5) is same as Reaction (1) and represents reduction of

MnO, after subtracting Reaction (3) from (4), it also provides the Gibbs
free energy equation for the reduction reaction of MnO.
∆G = -574,881.6 + (340.16) T;
0
Eq. (2)
At T = 1690.0K = 1417 C, ∆G = 0
0 0

It is clear from Eq. (2), that in order to reduce MnO into Mn the
0
operating temperature has to be more than 1417 C, so that Gibbs free Figure 2. Particle size distribution for Graphite, Coal and Bentonite
energy is negative and the reduction reaction for MnO can move in the sample (80% particle size for graphite, coal and bentonite 201.07 μm,
forward direction. The same conclusion we can also be drawn using an 46.23 μm, and 14.23 μm respectively)
Ellingham diagram. Ellingham diagrams are graphs between Gibbs
free energy and temperature, shown in Figure 1 (Webtool, 2009).

Figure 1. Ellingham diagram plotted between Gibbs free energy and
temperature for MnO, thermodynamically operating temperature to
0
reduce MnO should be higher than 1690K (1417 C)
MATERIALS AND PROCEDURES
As a source for manganese and iron, manganiferous iron ore was
used, bentonite was used as a binder. Graphite, polyethylene and coal
were used as reducing agent to produce four different types of pellets.
Pure graphite (99.9%) from Alfa Aesar was received in powdered
form and it was ground at Michigan Tech to reduce the 80% particle
size passing 201.07 μm. Polyethylene (C2H4) was used as source of
hydrogen for the self reducing pellets. It was received from Sigma-
Aldrich in powdered form 100% particle size passing 180 μm and was
utilized as received.
The bentonite clay was obtained from a nearby iron ore
concentrator, which was the same material that the plant was using as
the binder for their conventional concentrate pellets. The bentonite was
provided in dry powder form, and it had a plate water absorption
(PWA) value of 1000 +/- 50. Microtrac laser particle size analyzer was
used to determine the particle size to be 80% passing 14.34 μm. The
particle size distribution is shown in Figure 2. The coal was a steam
coal obtained as coarse lumps from a nearby power plant. It was a
blend of sub-bituminous coals from Antelope Mine, Wyoming and
Spring Creek Mine, Montana. The proximate analysis of the coal was:
12.51% of oxygen, 26.5% Moisture, 5.97% Ash, 0.20% Sulfur, 31.15%
Volatiles, 37.00% Fixed Carbon, and 8,800 BTU/lb. The coal was rod-
milled to 80% passing 46.23 μm for use in the experiments.
Manganiferous iron ore sample used for this experiment was
received in the form of rocks. It was initially crushed and ground at
Michigan Tech to 100% particle size passing 25μm size for the
chemical analysis. X-ray diffraction detected goethite (α-Fe.O (OH)),
hematite (Fe2O3), silica (SiO2), and calcium carbonate (CaCO3), as
shown in Figure 3.
Figure 3. X-ray diffraction pattern for manganiferous iron ore
Manganese oxide peaks did not appear in the X-ray diffraction,
because it was present in the amorphous form. The chemical analysis
of the ore was done at Michigan Tech University and is shown in Table
1. The manganiferous iron ore sample was also studied for liberation
size. Different size fraction of ore was mounted in epoxy, polished and
examined microscopically to determine the liberation size. The
manganiferous ore was divided into twelve samples using a rotary
splitter. Each sample was then wet ground in a rod mill to 100%
passing 25 μm and after drying sample was used directly to produce
four types of different pellets.
Table 1. Manganiferous iron ore composition.
Parameters % Wt Analytical Method
Fe 41.26 +/- 0.65 Dichromate titration
SiO2 5.10 +/- 0.23 Acid-insoluble Silica
Atomic absorption
Ca 3.80 +/- 0.16
spectroscopy
Mn 8.52 +/- 0.11 UV-Vis Spectrophotometry
Pelletization Process
To observe the effect of pellets’ composition on manganese oxide
reduction, four types of pellets with different compositions were
produced. To minimize the partial pressure of carbon monoxide (CO)
so that reduced metal manganese does not reoxidize, 99.9% pure
graphite was used as major reducing agent in “Pellet #1”. Polyethylene
((CH2) n). Pellet #2 was made using only polyethylene as major
reducing agent, to determine the effect of polyethylene alone on
manganese oxide reduction. To determine if polyethylene is necessary
at all for manganese oxide reduction “Pellet# 3” was made using only
graphite and no polyethylene. To compare the effect of these three
different pellets’ composition (“Pellet #1”, “Pellet #2”and “Pellet #3”),
traditional pellets were also made using coal and called “Pellet #4”.
Some preliminary experiments were completed in order to determine

2 Copyright © 2010 by SME

 SME Annual Meeting
Feb. 28-Mar. 03, 2010, Phoenix, AZ
° °
the composition of the pellets. Compositions of all these pellets are furnace was varied from 1425 C to 1450 C, and residence time was
shown in Table 2. varied from 20 to 40 minutes. All the experiments were repeated four
times to confirm the reproducibility of the results.
Table 2. Pellets' composition of “Pellet #1” (Graphite was used as
reducing and polyethylene was used as hydrogen source), “Pellet #2”
(Polyethylene was used as reducing agent), “Pellet #3” (Graphite was
used reducing, no hydrogen source was provided) and “Pellet #4”
(Traditional pellets, coal was used as reducing agent)
Manganiferous
Pellet Graphite Polyethylene Coal Bentonite
iron ore
type (%) (%) (%) (%)
(%)
Pellet# 1 87.00 10.34 2.00 -
Pellet# 2 85.00 - 14.34 -
0.66
Pellet# 3 87.00 12.34 - -
Pellet# 4 84.00 - - 15.34

A pelletizing drum with the following procedure was used to

combine the magnetite and reductant into pellets
1. The ore sample, binder and reducing agent were weighed and
mixed together thoroughly in a kneader mixer.
2. Then the mixture was delumped by forcing it through an 2.8 mm
(8-mesh) size screen
3. pelletizing drum at 25 rpm was used to produce pellets sized Figure 4. Optical microstructure of manganiferous iron ore sample of
between 11.2 mm and 12.7 mm less than 270-mesh particle size fraction embedded in epoxy and
° polished. The opaque iron oxide minerals are reflective, while the
4. Pellets were dried at 105 C for 24 hrs before using them to
translucent gangue mineral is darker and are not well-liberated
produce iron nuggets
Upon firing, pellets self reduced to produce pig iron nugget and
Reduction Process impurities in form of slag. Due to low iron content (41.26%) in ore
To observe the effect of furnace temperature was varied from sample, upon melting the iron coalesced into small metallic beads,
0 0
1425 C to 1450 C and residence time was varied from 20 to 40 instead of producing one big nugget. In case of “Pellet# 1”, the slag
minutes. For firing process two types of furnace were used. Pellets produced was green in color and crumbled upon cooling, shown in
were first placed on granulated petroleum coke bed in a clay-graphite Figure 5.
0
crucible and then this crucible was preheated in 1000 C pre-heated
muffle furnace for 7 minutes. The preheated crucible was then
transferred to a laboratory scale high temperature furnace where it was
0 0
heated further to either 1425 C or 1450 C for desired residence time.
The crucible was then removed from the furnace and air cooled
naturally to room temperature.
Chemical Analysis
When iron nugget and slag in the crucible was cooled down, iron
nuggets were separated from slag using a spex mill (a small vibrating
mill). Slag was ground and analyzed for the manganese content using
UV-Vis spectrophotometer.
Apparent density is measurement of mass per unit volume. In
case of pig iron nugget, apparent density represents the degree of
metallization, porosity of nugget, and slag separation (Anameric and
Kawatra, 2006). Apparent density of iron nugget produced was
determined using Archimedes’s principle; volume of displaced water
method (ASTM B 311-93, 2002). Pig iron nugget with high apparent
density indicates increase in metallization, decrease in porosity, and
increase in degree of slag separation (Anameric and Kawatra, 2006).
Since high apparent density is one of the important properties of high
quality of iron nugget, it was used to check the quality of iron nugget.
Figure 5. Iron nuggets and green powdered slag produced from
RESULTS AND DISCUSSION "Pellet# 1" (Graphite was used as reducing agent and polyethylene
0
was used to provide hydrogen source) at furnace temperature 1450 C
Liberation study for 30 minutes residence time
Liberation size study of the ore sample was also carried out. The
iron ore samples of different size fraction were mounted in epoxy, Manganese content in slag and iron nugget density at different
polished and etched. experimental conditions is shown in the Table 3. Results show that
manganese content in slag decreases with an increase in temperature
°
Optical micrograph of the iron ore sample for particle size fraction and residence time. When the pellets were fired at 1425 C for 20
53 µm (-270-mesh) is shown in Figure 4. It is clear from the figure that minutes, the percent manganese present in the slag was 22.16 +/-
iron oxide particles were not liberated from gangue minerals at 100% 0.69. But, when residence time was increased to 30 minutes,
particle size passing 53 µm. manganese content decreased in slag. Both increasing temperature
and increasing residence time resulted in more of the manganese
Pellet# 1
leaving the slag. Increase in temperature, decreased the manganese
Graphite as Major Reducing Agent and polyethylene used as amount in slag markedly for same residence at different temperature.
hydrogen source Temperature was more effective than residence time.
To study the reduction process, the operating temperature of
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 SME Annual Meeting
Feb. 28-Mar. 03, 2010, Phoenix, AZ
0 0
Temperature1425 C is not much higher than 1417 C; Gibbs free
energy is still very low at that temperature.
Table 1. Percent Mn present in slag from “Pellet# 1” made using
graphite as major reducing and polyethylene as hydrogen source, fired
at temperature 1425°C and 1450°C, residence time varied from 20 to
40 minutes
Iron Nugget
Temp., Residence % Mn present
Reductant Density
°C Time, min. in slag 3
(g/cm )
20 22.16 +/- 0.27 6.98 +/- 0.13
1425 30 10.34% 20.94 +/- 0.34 7.17 +/- 0.09
40 Graphite 17.98 +/- 0.11 7.26 +/- 0.07
20 2% 13.83 +/- 0.73 7.11 +/- 0.05
1450 30 Polyethylene 9.57 +/- 0.09 7.29 +/- 0.07
40 7.00 +/- 0.34 7.35 +/- 0.10

Pellet #2 Figure 6. Graphical representation of iron nugget apparent density

Polyethylene as Major reducing Agent, no graphite with increasing residence time for "Pellet# 1" (87% manganiferous iron
Same experimental conditions were utilized for the reduction ore, 10.34% graphite, 2% polyethylene, and 0.66% bentonite)
process of pellets made using polyethylene. Results are shown in
Table 4. In this case, the increase in temperature and residence time
does not show any effect on Mn content present in slag. It is clear from
the results that major content of manganese was going into slag. When
0
pellets were kept inside the muffle furnace at 1000 C, high volume of
smoke was observed. Polyethylene, ((C2H4)n) decomposes at low
temperature, before the reactions were started, most of C2H4 was lost
in smoke and there was not sufficient reducing agent left to complete
the reactions. This could be one of the major causes of Mn remaining
in the slag.
Table 2. Percent Mn and Fe present in slag from “Pellet #2” made
using polyethylene as major reducing, fired at temperature 1425°C and
1450°C, residence time varied from 20 to 40 minutes
% Mn Iron Nugget
Temp., Residence
Reductant present in Density
°C Time, min. 3
slag (g/cm )
30.69 +/-
20 7.21 +/- 0.12
0.63
1425 30.56 +/-
30 7.14 +/- 0.09
0.39
Figure 7. Iron nuggets and slag produced from "Pellet# 2"
30.02 +/- 0
(polyethylene used as reducing agent) at furnace temperature 1450 C
40 No Graphite, 6.99 +/- 0.21
0.93 for 30 minutes residence time
14.34%
Polyethylene 28.94 +/-
20 7.31 +/- 0.16
0.28
1450 27.99 +/-
30 7.21 +/- 0.13
0.92
26.70 +/-
40 7.17 +/- 0.05
0.81

Also with increase in residence time, there was slight decrease in

the apparent density of the iron nuggets produced. In order to figure
what was actually happening there, additional analyses were run. Slag
0
produced from the pellets fired at furnace temperature 1450 C for
residence time varied from 20 to 40 minutes, was analyzed for iron
content. For the residence time 20 minutes 7.06 +/- 0.27% iron was
present in slag and for residence time 40 minutes the percent iron
present in slag was 7.60 +/- 0.88%. This indicated that even though
there is slight decrease in apparent density with increase in residence
time, there was not much iron going into slag even for 40 minutes
residence time. Approximately, only 1.6% of iron was going into slag Figure 8. Graphical representation of iron nugget apparent density
from the initial pellets for all the residence time and at temperature of with increasing residence time for "Pellet# 2" (85% manganiferous iron
0
1450 C. Graphical representation of residence time vs. apparent ore, 14.34% polyethylene and 0.66% Bentonite)
densities of nugget produced is shown in Figure 6.
Pellet #3
Slag produced in this experiment was slightly shiny inside, slag Only graphite was used as major reducing agent, no hydrogen
0
and iron nugget produced at temperature 1450 C for 30 minute source was provided
residence are shown in Figure 7. Polyethylene was added to the “Pellet #1” (Pellet composition:
87% manganiferous iron ore sample, 10.34% graphite, 2%
polyethylene and 0.66% bentonite) to provide hydrogen in order to

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 SME Annual Meeting
Feb. 28-Mar. 03, 2010, Phoenix, AZ

reduce the partial pressure of generated carbon monoxide (CO) during Table 4. Percent Mn present in slag from “Pellet# 4” made using coal
reduction, so that CO does not interrupt with the manganese oxide as major reducing, fired at temperature 1425°C and 1450°C, residence
reduction process. It was also area of interest to determine if providing time varied from 20 to 40 minutes
hydrogen source is helping or not. “Pellet #3” was made to test the Iron Nugget
requirement of adding polyethylene (as hydrogen source) in the Temp., Residence % Mn present
Reductant Density
pellets, 2% polyethylene was added to “Pellet #1” to provide hydrogen °C Time, min. in slag 3
(g/cm )
source, this amount was replaced by graphite and pellets’ composition 20 31.60 +/- 0.66 6.99 +/- 0.19
for “Pellet #3” was 87.00% manganiferous iron ore, 12.34% graphite
1425 30 15.34% Coal 30.42 +/- 0.44 7.09 +/- 0.13
and 0.66% of bentonite. For the reduction process, the pellets were
0
only fired at furnace temperature 1450 C (Since in previous 40 No graphite or 30.65 +/- 0.48 7.14 +/- 0.11
0
experiments temperature 1425 C was not sufficient to reduce 20 polyethylene 30.36 +/- 0.72 7.04 +/- 0.22
manganese oxide into manganese). Residence time was varied from 1450 30 was added 29.08 +/- 0.43 7.23 +/- 0.09
20 to 40 minutes. Results are shown in Table 5. 40 29.22 +/- 0.93 7.25 +/- 0.11
Table 3. Percent Mn present in slag from “Pellet #3” made using only
graphite (no hydrogen source was provided using polyethylene) as
major reducing, fired at temperature 1450°C, residence time varied
from 20 to 40 minutes
% Mn Iron Nugget
Temp., Residence
Reductant present in Density
°C Time, min. 3
slag (g/cm )
22.83 +/-
20 6.92 +/- 0.18
1.38
12.34%
1450 Graphite, No 19.84 +/-
30 7.00 +/- 0.13
polyethylene 0.62
15.95 +/-
40 7.23 +/- 0.18
0.99

The amount of manganese going into slag is lower than “Pellet

#2” but it is higher than “Pellet #1”, this indicates adding 2.00%
polyethylene was sufficient and necessary in order to reduce
manganese oxide. This also validates the previously mentioned first
thermodynamic condition of reducing partial pressure of CO. The slag
produced in this experiment had green color which indicated low iron
content in slag and it did not crumbled upon cooling. The graphical Figure 10. Graphical representation of iron nugget apparent density
representation of the residence time vs. apparent density is shown in with increasing residence time for "Pellet #4” (84.00% manganiferous
Figure 9. iron ore, 15.34% coal, and 0.66% bentonite)

Figure 9. Graphical representation of iron nugget apparent density

with increasing residence time for "Pellet #3”
Pellet #4
Traditional pellets made using coal
To compare the effect of different pellets’ composition traditional
pellets were made using coal. Pellets’ composition was 84.00%
manganiferous iron ore, 15.34% coal and 0.66% bentonite.
The results are shown in Table 6. Results from traditional pellets
shows the same trend as pellets made using polyethylene showed.
There was no effect of operating temperature and residence time on
manganese content going into slag.
Figure 11. Mn content in slag with increasing residence time and at
0 0
temperature 1425 C and 1450 C for “Pellet #1”, "Pellet #2", “Pellet
#3”and “Pellet #4” (the error bars are very small to be appear clearly in
the figure).
CONCLUSION
From the results, following conclusions were drawn:
1. In order to reduce manganese, the pellets should be fired at
temperature of 14500C and a low partial pressure of CO is
required. Also, in order to reduce manganese oxide higher
temperature was more important than residence time.

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 SME Annual Meeting
Feb. 28-Mar. 03, 2010, Phoenix, AZ

2. Adding 2.00% polyethylene to provide hydrogen source as a 15. Yastreboff M., Ostrovski O. and Ganguly S., Effect of gas
supplement to graphite reductant was sufficient to reduce composition on the carbothermic reduction of manganese oxide.,
MnO. However, when only polyethylene was used, it did not ISIJ International, Vol. 43, 2003, No. 2, pp. 161-1
help in MnO reduction. This could be because when the only
reductant was polyethylene, most of the reducing agent was
lost in the smoke in the beginning of the reduction process.
As a result there was not sufficient amount of reductant left
to complete the reaction and resulted more manganese ends
up in slag.
3. Providing hydrogen source inside the pellets helped with
MnO reduction process compared to pellets containing no
hydrogen source.
4. The fraction of manganese that remains in the slag can be
effectively controlled through manipulation of temperature,
quantity of reductant, and inclusion of a hydrogen source.
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