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Morphology and reduction kinetics of fluxed
iron ore pellets
S. Prakash, M. C. Goswami, A. K. S. Mahapatra, K. C. Ghosh, S. K. Das,
A. N. Sinha, and K. K. Mishra
slag than in the case of the externally uxed iron ore pellet,
impurity reversal to the metal is expected to be minimised
The present paper describes studies of the
during smelting.1 The slag would essentially oat o the
reduction and sintering behaviour, followed by
assimilated impurities.
examination of the structural changes taking place,
Iron ore pellets are commonly used as an alternative
during direct reduction of fluxed composite (ore
starting material in conventional as well as comparatively
plus coal) pellets. The kinetics and morphological
new iron- and steelmaking processes. Attempts have recently
aspects of the direct reduction of fluxed composite
been made to employ internal reductants and uxes to
pellets are compared with those for the gaseous
accelerate the reduction kinetics without aecting the physico-
reduction of fluxed ore pellets without carbon
chemical properties of the pellets.13 The reduction strength,
addition. It is shown that the chemical reaction is
however, depends largely on the precipitation behaviour of
the rate limiting factor for fluxed composite pellets,
iron on wustite (FeO
x
) during reduction.4 Earlier authors4,5
and the mass transport of reactant gas through the
have discussed some aspects of the reduction and sintering
reaction product iron layer governs the overall
behaviour of uxed pellets. Prakash5 demonstrated signicant
reduction process in the case of fluxed ore pellets.
variation in the pore size distribution and changes in iron
Microscopic analysis of the fluxed composite
morphology during reduction.
pellets has indicated no tendency to form a
The gaseous reduction of iron ore lumps and pellets
reduction inhibition iron shell towards the end of
has been extensively studied, discussed, and reported in the
the reduction, as found in the case of gaseous
literature. Based on several investigations611 into the gaseous
reduction of fluxed ore pellets under identical
reduction of iron oxide, the rate determining mechanism
reduction process conditions. The effects of
has been described either as the interparticle gaseous diusion
basicity, Fe/C, temperature, and other variables on
through the reduced layer or as the chemical reaction at
morphological and microstructural changes in the
the interface between the reduced and unreduced layers.
directly reduced fluxed composite pellets have been
The extent of reduction and the structural changes depend
experimentally investigated in the present work.
on several operating variables.8,1115 The most critical of
I&S/1422
these is gaseous diusion through the reduced layer, and
this depends upon the porosity of the pellets. Abraham and
The authors are at the National Metallurgical Laboratory,
Ghosh16 predicted a signicant mass transfer resistance in
Jamshedpur, India. Manuscript received 4 January 1999; accepted
the oxide. 5 May 1999.
Rao17 investigated the reduction kinetics of a mixture
2000 IoM Communications Ltd.
of hematite and carbon powders in the temperature range
8501087C. The reduction process can be described in terms
of the availability of carbon monoxide within the mixture.
Although some researchers have attempted to characterise
INTRODUCTION
the reaction mechanism and the rate controlling steps
Production of liquid iron outside the blast furnace has
mathematically, there is little experimental evidence based
attracted considerable attention during the past two decades.
on microscopic studies to suggest how temperature, carbon
The smelting reduction processes are intended to provide an
particle size, hematite/carbon ratio in the mixture, and
attractive alternative route to the conventional steelmaking
addition of catalysts, binders, and uxes aect the reduction
process. These processes, however, require very select grades
kinetics.
of raw materials. Both iron ore and coal must be fed in the
Investigation1821 into the interaction of CaO with Al
2
O
3
,
form of lumps of particular size. Fines of ore, Indian blue
SiO
2
, and FeO
x
have shown that dierent concentrations
dust, or coal nes produced during mining or crushing
of these compounds cause a change in iron morphology
cannot be used in these processes without agglomeration.
and result in dierent reduction conditions. According to
Although such nes can be directly used in uidised bed
the phase diagram of Philips and Muan,18 calcium diferrite
reactors, sticking problems during the reduction process
(CaO.2Fe
2
O
3
=CaFe
4
O
7
) is stable in the range 11551226C
cause numerous breakdowns. An alternative process is the
in air at 1 atm. Edstrom19 regarded this compound as the
direct reduction of iron ore pellets, using solid or gaseous
most important binding phase for the base sinter process.
reductants. However, during the smelting of these pellets,
A study20 of the eect of Al
2
O
3
on the formation of calcium
external reductant and uxes must be added to reduce the
deferrite has shown that Al
2
O
3
decreases the melting temper-
residual oxygen content of the iron oxide in the molten slag, ature, which enhances the formation of calcium diferrite.
and to give the necessary assimilation of impurities such as As is the case with CaO, it is not possible to reduce SiO
2
sulphur, phosphorus, and vanadium, thereby generating slag in the temperature range 6001000C. In contrast to CaO,
of suitable composition for the furnace lining, respectively. SiO
2
can only formthe chemical compound fayalite (Fe
2
SiO
4
),
The concept of the directly reduced uxed composite pellet which cannot normally be reduced by CO. Thus, SiO
2
can
implies that the uxes and carbonaceous materials added be referred7,18 to as a sluggish compound, which hinders
to the iron ore pellet feed would generate a slag of suitable the reduction of iron oxide. The apparent deviation can
composition and adequate reduction potential in a bath be attributed to the local oxygen potential at which the
smelting process. As the impurities bound in the uxed FeSi
2
O
4
was formed, and hence which diered from that
of the ambient atmosphere. composite pellet FCP can be more easily assimilated in the
ISSN 03019233 194 Ironmaking and Steelmaking 2000 Vol. 27 No. 3
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Prakash et al. Reduction of fluxed iron ore pellets 195
The reduction reaction in ore plus coal pellets at high
temperature is rather complex. It involves22 devolatilisation
of coal and reduction via CO and hydrogen in the volatiles,
reduction via hydrogen and carbon generated by cracked
hydrocarbons in the volatiles, and true direct reduction
and reduction via gaseous intermediates.
The pellets should be tested to determine properties such
as porosity, green strength (impact test), isothermal reduction
characteristics, reduction strength, compressive strength after
reduction (CSAR), and sticking characteristics. Another
important factor to consider during reduction in the shaft
is clustering, which can result in uneven gas distribution
during discharge. The standard test methods23,24 are rather
inaccurate, oversimplications of the process steps and
treatments carried out under simulated conditions. There
is a danger, therefore, of optimising the behaviour of an
ore product under test conditions rather than its properties
under actual process conditions.
To minimise smelting costs, it is essential that the directly
reduced iron is highly metallised.25 An easily reducible
burden is necessary to achieve this without sacricing high
productivity in the direct reduction furnace. The limiting
factor is usually the shape of the reduction curve towards
the end of the reduction process. The time required to attain
1 Schematic diagram of experimental setup for reduction
the limiting value of reduction can, however, be minimised of pellets
by the use of suitable uxes and additives.
The purpose of the present study was to evaluate on a
laboratory scale the sintering and reduction characteristics
Apparatus and procedure
of uxed composite (ore plus coal ) pellets for use in direct
The reduction experiments were carried out in a resistance reduction and smelting reduction processes. Directly reduced
heated vertical tube furnace (Fig. 1). The directly reduced iron pellets were produced by the simultaneous reduction
uxed composite pellets were made using various pro- and sintering of uxed composite pellets which comprised
portions of Indian blue dust, reductants, lime, and an a mixture of ore plus coal nes, uxes, and a suitable
organic binder. The particle size of all the materials was binder. It was found that, for uxed composite pellets, the
200 mesh (0074 mm). The CO generated in situ served chemical reaction was the rate controlling step, described
to maintain a reducing atmosphere inside the furnace. The by a ln(1a) type equation, where a is the degree of
pellet samples were heated to predetermined reduction reduction. The kinetics of uxed ore pellets made without
temperatures of 1073, 1173, 1273, and 1323 K for a specic carbon addition, however, indicated diusion controlled
reduction time. The reduced samples were then cooled in rate phenomena. In the present work the main process
nitrogen, weighed, and kept in a vacuum desiccator before parameters to aect the kinetics and the iron precipitation
chemical analysis and microscope studies. characteristics during pellet reduction, i.e. temperature,
Experiments were carried out to study the eects of Fe/C, reduction gas potential, and reduction time, have been
temperature, non-ferrous oxide content, Fe/C ratio, addi-
experimentally investigated. The reduction mechanisms and
tives, and basicity on the reduction and strength charac-
morphological changes for both uxed ore pellets and
teristics of the pellets. Some additional isothermal reduction
uxed composite pellets are described.
experiments were carried out to study the iron precipitation
behaviour during reduction. Identical pellet samples were
EXPERIMENTAL
heated to the temperatures of 1073, 1173, and 1273 K for
Raw materials and chemical compositions
a xed duration of 45 min. The reacted pellets were removed,
quenched by nitrogen gas, fractured, and then analysed Both uxed iron ore and uxed composite ore plus coal
types of pellets were made and tested in the laboratory using SEM.
The reduced and sintered pellets were tested for compressive using equipment and methods developed at the National
Metallurgical Laboratory, Jamshedpur, India. Blue dust strength, porosity, and extent of reducibility. All the tests
were performed on pellets which were within the diameter was used in the preparation of these pellets. Chemical
compositions of the blue dust, coal, and ux are given in range of 10125 mm. To compare the reduction mechanisms
of uxed iron ore ( blue dust without internal reductant Table 1. Organic binder was used during balling to minimise
the quantity of acid gangue. pellets) and uxed composite (with internal reductant) pellets,
isothermal gaseous reduction of uxed ore pellets under Pellets were produced in a rotary conical drum. Their
strength characteristics, showing the ability to withstand similar experimental conditions was carried out. In this test
a CON
2
mixture (30 : 70) was passed through the bed; handling during transportation, were evaluated by impact
drop test.4 reduction temperatures of 1073, 1273, and 1323 K were,
Table 1 Chemical compositions* of raw materials, %
Raw material Fe
T
Fe
2
O
3
SiO
2
Al
2
O
3
CaO MgO S P LOI FC VM Ash
Blue dust 683 976 134 040 013 002 055
Lime Traces 054 060 80 080 858
Non-coking coal 49 385 125
ash 24 428 292 230 18 Traces 0005
* Fe
T
total Fe; LOI loss on ignition; FC fixed carbon; VM volatile matter.
Proximate analysis.
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196 Prakash et al. Reduction of fluxed iron ore pellets
(a)
(b)
(a)
(b)
a B
2
=082; b B
2
=133
a from Fig. 2a; b from Fig. 2b
2 Kinetic data for reduction of fluxed composite pellets
3 Kinetic analysis using modified kinetic data for fluxed
composite pellet reduction
however, the same as in the former case. Tests carried out
Figure 5 shows analysis of the reduction kinetics for the
according to the Bureau of Indian Standards for evaluating
isothermal gaseous reduction of uxed ore pellets ( basicity
iron ore and pellets are discussed in detail elsewhere.24
of 133). Curves for the fraction of the pellets reacted, i.e.
the fraction of oxygen removed, against time at the temper-
atures of 1073, 1173, 1273, and 1323 K are shown in Fig. 5a.
RESULTS AND DISCUSSION
It can be seen that the reduction rate decreases gradually
Reduction kinetics with time and with an increase in fraction reacted. With
the progress of reaction, therefore, some changes seemingly Typical results for the reduction kinetics of uxed iron
tend to retard the rate of reduction. The CrankGinstling ore plus coal pellets are shown in Fig. 2 for basicities of
082 and 133. The curves do not pass through the origin
because the reaction mass underwent a short heating period
to attain the preset temperatures, i.e. time t=0 is ill dened.
However, all curves have the same intercept, indicating
consistency in results. The degree of reduction a, i.e. degree
of oxygen removal, and reduction time t values for the
kinetic curves must be extrapolated accordingly. It was
assumed, however, that no reaction had taken place during
the rather short heating period and a modied time, i.e. the
time when the pellet mass attained the specic temperature,
was used for kinetic analysis. The resulting isothermal
kinetic data using the modied times for the reduction
experiments on the pellets are shown in Fig. 3.
A good linear relationship was obtained between the
modied time and G(a), where G(a) =ln(1a). This
interpretation serves only as indirect proof that a solution
loss reaction occurs between the CO
2
and carbon particles
within the pellets, and that it governs the overall reduction
process. The kinetic data t approximately a rst order rate
equation (Fig. 3). The rate constants determined from Fig. 3
t an Arrhenius type equation as shown in Fig. 4, and yield
activation energy E values in the ranges 4950 kJ mol1
and 4752 kJ mol1, respectively, for basicities of 082 and
133. As the CO
2
carbon reaction is an activation controlled
chemical reaction, the direct reduction component is signifi-
cant in the reduction of composite pellets. The validity of
the model has been tested using the dierential approach,6
resulting in E values nearly the same as those obtained
(a)
(b)
using the integral approach. The results indicate that a
a B
2
=082; b B
2
=133
higher basicity enhances the reduction kinetics, although
4 Evaluation of activation energy E of fluxed composite
the reaction mechanism remains the same within the range pellet reduction using differential and integral
approaches of basicities (082133) investigated in the present work.
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Prakash et al. Reduction of fluxed iron ore pellets 197
(a)
(b)
a B
2
=082; b B
2
=133
6 Dependence of reduction time onreductiontemperature
of fluxed composite pellets
The test results show that the characteristics of the
uxed composite pellets depend both on their total content
of non-ferrous oxides (CaO, SiO
2
, Al
2
O
3
, etc.) and on the
composition of these oxides. Hence, it may not be possible
to obtain certain properties of the pellets simply by
prescribing their basicities B
2
=%CaO/%SiO
2
.
In the present case, blue dust, coal, and basic additives
were used; the quantity of non-ferrous oxides increases in
proportion to the CaO content. For all mixes the following
(a)
(b)
(c)
5 a Isothermal kinetic data for reduction of fluxed relationship holds approximately: % non-ferrous oxides
pellets, B
2
=133; b kinetic analysis of reduction of
(non-FeO
x
) =constant+%CaO.
fluxed pellets using data from Fig. 5a; c evaluation
Figure 7 shows the dependence of non-FeO
x
contents of
of activation energy using differential and integral
the composite pellets on reduction time at various levels
approaches for rate controlling steps, from Fig. 5b
of degree of reduction. Interestingly, a higher non-FeO
x
content in the pellets enhances the rate of reduction. It
Brounshtein5,6 equation indicates that product layer diusion
can be inferred from this that the lime addition enhances
is the overall rate controlling step (Fig. 5b). This may be
the rate of reduction. Figure 8 shows that while the green
ascribed to the formation of a CaOFeOSiO
2
phase. The
strength is fairly independent of the coal quantity (030%),
uxed pellets without an internal reductant tend to form a
an increase in both lime and organic binder additives
reduction restraint product layer, which retards the rate of
signicantly increases the impact strength of the pellet. In
reaction. The transport of reaction gas through the product
Fig. 9, porosity and CSAR are plotted against temperature.
layer is a diusion controlled reaction. The mass transfer
The extra lime addition ( higher basicity) surprisingly gives
limitations modify the rate, yet this does not inuence
the activation energy signicantly. Thus, a high activation
energy (4246 kJ mol1) exists despite partial control of mass
transfer (Fig. 5c). To achieve a higher degree of reaction
rate, it is necessary to minimise the inhibiting eect of this
resistance by appropriate process control, or a measure
such as increasing the area of the reacting surface. It is also
implied by the above that if uxed composite pellets of ore
plus coal can be used, the process rate can be enhanced by
at least an order of magnitude.
Factors influencing pellet characteristics
Figure 6 shows typical results for the dependence of
reduction time on the reduction temperature, indicating
that the time needed to achieve a given degree of reduction
decreases with an increase in reduction temperature. At
7 Dependence of reduction kinetics on non-ferrous
higher temperatures, however, an increase in basicity seems oxides (non-FeO
x
) in fluxed composite pellets: B
2
=133,
T=1323 K to cause a slight decrease in the temperature dependency.
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198 Prakash et al. Reduction of fluxed iron ore pellets
8 Effects of additives on green strength of fluxed
composite pellets
only a marginal decrease in porosity within the range investi-
gated. A higher lime addition and increase in reduction
temperature apparently decrease the porosity, and they
signicantly increase the CSAR. As is well known, the degree
of agglomeration increases with an increase in temperature,
leading to lower porosity and generally higher strength, as
indeed appears to be the case from Fig. 9. Furthermore, it
is apparent that the porosity decreases more rapidly with
an increase in temperature at higher lime additions. The
temperature dependence of the CSAR is fairly dependent
on an increase in the lime addition. At higher temperatures
the lime additions seem to cause a reasonable increase in
CSAR dependency on the temperature.
Microscopic analysis
In gaseous reduction of uxed ore pellets, one reactant gas
is transferred from the bulk gas stream and diuses between
the grains through a solid reaction product layer. In the
present work, the reduced uxed ore pellets were examined
using a Nikon optical microscope. Figure 10a depicts the
formation of a dense iron shell around the surface. It is
interesting to note, however, that the reaction appears to
proceed from the outside towards the centre for each grain,
a
b
(c)
10 Optical micrographs depicting a tendency of iron
shell formation during reduction of fluxed pellets,
100; b dense iron shell surrounding grains of fluxed
pellets, 50; c schematic diagram of grain model
forming a dense iron shell around the grain (Fig. 10b).
Further growth of the iron shell occurs along a direction
perpendicular to the iron/wustite interface and produces
typical morphological changes, which are shown schematically
in Fig. 10c. The shelled wustite is converted to iron by the
neighbouring iron nuclei via solid diusion. The reduction
retardation noted above may be a result of slow diusion in
the solid phase. The dierence in the degree of reduction
between two successive time intervals on the reduction time
curve (Fig. 5a) indicates that the rate of reduction decreases
with the progress of reduction. The cause of such a retardation 9 Dependence of compressive strength after reduction
(CSAR) and porosity on temperature may be the binding of iron oxide in the acid slag phase or
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Prakash et al. Reduction of fluxed iron ore pellets 199
a
b
a highly reduced; b densely sintered
11 Optical micrographs revealing microstructure of
fluxed composite pellets 200
the formation of dense iron shells around the remaining
a
b
c
wustite particles. If reduction stops around or before achieve-
a whisker, 1173 K; b porous, 1273 K; c dense, 1323 K
ment of a degree of reduction in pellets with a high iron
12 Microstructures of fluxed reduced iron pellets showing
content, the main reason most probably is the formation
morphological changes at given temperatures
of iron shells, which hinders the ingress of reduction gas to
the inside core. The formation of the dense iron shell is the
major cause of retardation of the reduction rate observed magnication is kept about four times higher than that of
Figs. 12b and c so that the whisker morphology is clearly at the nal stage of reduction. These results correlate with
the shape of the reduction curve (Fig. 5a). This retardation visible. In addition, increased mass transfer rates are possible
in composite pellets owing to hydrocarbon liberation at may also hinder the sintering process.
Figure 11 shows optical micrographs of reduced FCPs, low temperatures between 200 and 600C (Ref. 22) and the
inuence of H
2
/H
2
O via the gaswater shift reaction when revealing microstructures of highly reduced and densely
sintered iron particles ( bright contrast) and agglomerates using coal with a high volatiles content (Table 1). These
reactions can aect the microstructure of the oxide grain of ne carbonaceous particles. It is interesting to note that,
despite the incomplete reaction of carbon and lack of full by the introduction of defects and have the generation of
new paths for the reaction gases along grain boundaries. densication, the CSAR typically approaches 115 kg/pellet
(Fig. 9). This can probably be ascribed to the formation of However, the interrelationships of these various precipitation
behaviours is rather complex. calcium ferrites, primarily diferrites, which during reduction
form a calciferous wustite that is readily reduced despite Typical SEM images of fractured reduced pellets, obtained
with a Jeol 840 scanning electron microscope, are shown its low swelling.
Microscope studies of reduced xed composite pellets have in Figs. 13 and 14, depicting the eect of residence time
and temperature, respectively, on changes in microstructure revealed some interesting results of sintering, discussed below
in association with the reduction results. Figure 12 shows of the pellets. It can be seen that, with an increase in time
and temperature, the ferrite phase tends to grow on a brous (Fig. 12a), porous (Fig. 12b), and dense (Fig. 12c)
iron growth of the uxed composite pellets during reduction substrate of wustite, progressively producing bridges, which
consolidate and produce aggregate particles. The reaction at temperatures 1073, 1173, and 1273 K, respectively, i.e. in
steps of 100 K. These results indicate three kinds of iron may initially proceed by the diusion of interstitial carbon
into the matrix of ore iron oxide, becomes propagated precipitation, which are seemingly governed by the temper-
ature and the corresponding reduction potential during by interfacial reaction gas expulsion and reaction with
iron oxide, and is then followed by shrinkage during iron the reduction process. The visual dierences could also be
attributed to thermal expansion in the pellets, and variations precipitation at the hypostoichiometric iron oxide FeO
x
layer. This may eventually cause pores to expand owing to in packing density during pelletisation. In Fig. 12a, the
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200 Prakash et al. Reduction of fluxed iron ore pellets
a
b
c
a 20 min; b 45 min; c 60 min
a
b
c
a 1173 K; b 1273 K; c 1323 K 13 Microstructural changes in fluxed composite reduced
iron pellets with increase in residence time: Fe/C=77, 14 Microstructures of fractured fluxed composite
B
2
=20, T=1323 K reduced iron pellets showing effect of temperature:
Fe/C=77, B
2
=20, T=60 min
internal gas pressure. These pores are further increased as
Figure 15 shows the eect of lime addition on the reduction
a result of the reduction of wustite to metallic iron.
characteristics of the pellets. The reaction rate was found
Figure 14 depicts the uid phase formation. The uid
to increase with higher lime addition. The SEM images in
phase presumably comprises an amalgamation of uid oxides
Fig. 15 indicate signicant changes in the morphology of
(slag: CaOFeOSiO
2
) and molten metal mass (reduced
iron precipitation owing to the presence of CaO, and this
wustite), which can drip o the wustite surface. It does not
must account for the change in reducibility. It is possible
close the pores, however, as the slag generally does not wet
that an increasing CaO percentage decreases the solubility
the carbon. It spreads quickly across the carbon particles
of FeO in the slag phase and inhibits fayalite formation.
owing to an apparent lowering of interfacial tension when
It is also fairly likely that additional CaO may change
the reactions take place. Subsequent transport of carbon into
the swelling behaviour and porosity thereby enhancing
the melt may occur via a dissolutionprecipitation reaction
reducibility, as CaO favours the nucleation of porous iron.
mechanism, in which the carbon precipitates out of the
slag phase and wustite/carbon interface. The dissolution of
CONCLUSIONS
carbon into the metallic fraction of the moment mass can
The reduction kinetics of uxed composite pellets obeys decrease the melt temperature, thereby resolidifying the
rst order type models, and shows a signicant dependence carbon decient iron phase and preventing dripping of the
on temperature. The overall rate of iron oxide reduction uid oxides. Further transport of carbon can also occur via
of uxed composite pellets is seemingly controlled by the solid state diusion through intermediate iron oxide in the
reduced ore layer, and the reduction continues. gasication of carbon by CO
2
and, being highly endothermic,
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Prakash et al. Reduction of fluxed iron ore pellets 201
described in the present work. It has been shown by SEM
that lime additions inuence the iron morphology and
enhance the reduction and strength properties of the pellets.
Binder is not seemingly a signicant parameter beyond a
certain value. However, this parameter is very important
in attaining the green strength of the pellets. This in turn
aects the compressive strength after reduction (CSAR) of
the pellets.
The range of carbon and CaO contents for which an
iron shell is likely to form depends on variables such as
the other gangue contents and the reduction temperature.
Therefore the optimum values for carbon and CaO contents
cannot be generalised. The reduction and simultaneous
sintering of the uxed composite reduced pellets is not a
linear continuum. It rather seems to be a disconnected and
discursive montage of overlapping phenomena.
ACKNOWLEDGEMENTS
The investigators wish to thank Professor P. Ramachandra
Rao, Director National Metallurgical Laboratory (NML),
Jamshedpur for permission to carry out this work and
for the use of NML facilities during the course of the
investigation.
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Ironmaking and Steelmaking 2000 Vol. 27 No. 3