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<a href=International Journal of Mineral Processing 99 (2011) 43 53 Contents lists available at ScienceDirect International Journal of Mineral Processing j o u r n a l h om e p a g e : www. e l s ev i e r. c om / l o c a t e / i jm i n p ro Effect of pellet basicity and MgO content on the quality and microstructure of hematite pellets Srinivas Dwarapudi ⁎ , Tamal K. Ghosh , Amitabh Shankar , Vilas Tathavadkar , D. Bhattacharjee , R. Venugopal R&D, Tata Steel Ltd, Jamshedpur, India FME, ISM University, Dhanbad, India article info Article history: Received 18 September 2010 Received in revised form 24 March 2011 Accepted 27 March 2011 Available online 1 April 2011 Keywords: Pellet induration Swelling Acid pellets Reduction degradation index Silicate melt MgO pellets abstract Quality of pellets is in fl uenced by the nature of ore or concentrate, associated gangue, type and amount of fl uxes added and their subsequent treatment to produce pellets. These factors in turn result in the variation of physicochemical properties of the coexisting phases and their distribution during pellet induration. In the present study, effect of pellet basicity and MgO content on the melt formation and microstructure during the induration was examined. Fired pellets with varying basicity (0 to 0.8) and MgO (0 and 1.5%) content were tested for cold strength, reduction degradation index, reducibility, swelling and softening – melting characteristics. Optical microscope studies with image analysis software were carried out to estimate the amount of different phases. SEM-EDS analysis was done to record the chemical analysis of oxide and slag phases. X-ray mapping was also carried out to understand the distribution of CaO, MgO, SiO and Al O in different phases. From the results, it was observed that with increasing basicity, RDI and softening – melting characteristics of pellets found to be improved. Addition of MgO to both acid and limestone fl uxed pellets considerably reduced their swelling tendency. Improved pellet quality could be attributed to the formation of suf fi cient amount of silicate melt in basic pellets and high melting point slag in MgO pellets. Limestone fl uxed pellets at 0.8 basicity, pyroxenite fl uxed pellets at 1.5% MgO and dolomite fl uxed pellets at 0.4 basicity & 1.5% MgO exhibited optimum metallurgical properties among all the pellets studied. © 2011 Elsevier B.V. All rights reserved. 1. Introduction Iron ore agglomerate quality plays a vital role in decreasing the reducing agent consumption and increasing the productivity of blast furnace. In most of the integrated steel works, the burden mix for blast furnace is decided as per the availability of the iron ore agglomerates like sinter and pellets. More attention has been given in recent years to the use of fl uxed pellets in blast furnace due to their good strength and improved reducibility, swelling and softening – melting charac- teristics. Generally, quality of pellets is in fl uenced by the nature of ore or concentrate, associated gangue, type and amount of fl uxes added and their subsequent treatment to produce pellets. These factors in turn result in the variation of physicochemical properties of the coexisting phases and their distribution during pellet induration. Hence properties of the pellets are largely governed by the form and degree of bonding achieved between ore particles and the stability of these bonding phases during reduction of iron oxides ( Panigraphy et al., 1990 ). ⁎ Corresponding author at: R&D, Tata Steel Ltd, Burma mines post, Jamshedpur, 831007, Jharkhand, India. Tel.: +91 6572148928 (Of fi ce), +91 9204058889 (mobile); fax: +91 65722717. E-mail address: srinivasd@tatasteel.com (S. Dwarapudi). 0301-7516/$ – see front matter © 2011 Elsevier B.V. All rights reserved. doi: 10.1016/j.minpro.2011.03.004 In fl uxed pellets, the bonding is achieved through silicate melt formation during induration. The amount of gangue in the concen- trate, CaO & MgO in the fl uxes and binder in fl uences the amount and chemistry of silicate melt. CaO fl uxes silicate melt as well as reacts with iron oxide to form different calcium ferrites. MgO either enters the magnetite lattice to form magnesioferrite or dissolves in the slag phase. These melting phases interact with each other and dissolve a variable amount of iron oxides. As the formation of phases and microstructure during induration depends on the type and amount of fl uxes added, there is a need to study the effect of these fl uxing agents in terms of CaO/SiO ratio and MgO content on pellet quality. Wynnyckyj et al. presented results of adding CaO in the form of lime on fi red pellet quality; they found addition of lime increases the pellet shrinkage and hence increase the pellet strength due to the formation of calcium silicate and calcium ferrites ( Wynnyckyj and Fahidy, 1974 ). Hamilton et al. revealed that CaO fl uxed pellets exhibit improved strength when fi red between 1200 °C and 1400 °C due to the formation of more slag in the porous structures and consolidation of the pellet. ( Hamilton, 1976 ). Panigraphy, S.C et al. presented detailed results of limestone and dolomite fl uxed pellets from hematite concentrate; in limestone fl uxed pellets silicate melt was the predominant bonding phase up to " id="pdf-obj-0-7" src="pdf-obj-0-7.jpg">

Contents lists available at ScienceDirect

International Journal of Mineral Processing

j o u r n a l h om e p a g e : www. e l s ev i e r. c om / l o c a t e / i jm i n p ro

<a href=International Journal of Mineral Processing 99 (2011) 43 53 Contents lists available at ScienceDirect International Journal of Mineral Processing j o u r n a l h om e p a g e : www. e l s ev i e r. c om / l o c a t e / i jm i n p ro Effect of pellet basicity and MgO content on the quality and microstructure of hematite pellets Srinivas Dwarapudi ⁎ , Tamal K. Ghosh , Amitabh Shankar , Vilas Tathavadkar , D. Bhattacharjee , R. Venugopal R&D, Tata Steel Ltd, Jamshedpur, India FME, ISM University, Dhanbad, India article info Article history: Received 18 September 2010 Received in revised form 24 March 2011 Accepted 27 March 2011 Available online 1 April 2011 Keywords: Pellet induration Swelling Acid pellets Reduction degradation index Silicate melt MgO pellets abstract Quality of pellets is in fl uenced by the nature of ore or concentrate, associated gangue, type and amount of fl uxes added and their subsequent treatment to produce pellets. These factors in turn result in the variation of physicochemical properties of the coexisting phases and their distribution during pellet induration. In the present study, effect of pellet basicity and MgO content on the melt formation and microstructure during the induration was examined. Fired pellets with varying basicity (0 to 0.8) and MgO (0 and 1.5%) content were tested for cold strength, reduction degradation index, reducibility, swelling and softening – melting characteristics. Optical microscope studies with image analysis software were carried out to estimate the amount of different phases. SEM-EDS analysis was done to record the chemical analysis of oxide and slag phases. X-ray mapping was also carried out to understand the distribution of CaO, MgO, SiO and Al O in different phases. From the results, it was observed that with increasing basicity, RDI and softening – melting characteristics of pellets found to be improved. Addition of MgO to both acid and limestone fl uxed pellets considerably reduced their swelling tendency. Improved pellet quality could be attributed to the formation of suf fi cient amount of silicate melt in basic pellets and high melting point slag in MgO pellets. Limestone fl uxed pellets at 0.8 basicity, pyroxenite fl uxed pellets at 1.5% MgO and dolomite fl uxed pellets at 0.4 basicity & 1.5% MgO exhibited optimum metallurgical properties among all the pellets studied. © 2011 Elsevier B.V. All rights reserved. 1. Introduction Iron ore agglomerate quality plays a vital role in decreasing the reducing agent consumption and increasing the productivity of blast furnace. In most of the integrated steel works, the burden mix for blast furnace is decided as per the availability of the iron ore agglomerates like sinter and pellets. More attention has been given in recent years to the use of fl uxed pellets in blast furnace due to their good strength and improved reducibility, swelling and softening – melting charac- teristics. Generally, quality of pellets is in fl uenced by the nature of ore or concentrate, associated gangue, type and amount of fl uxes added and their subsequent treatment to produce pellets. These factors in turn result in the variation of physicochemical properties of the coexisting phases and their distribution during pellet induration. Hence properties of the pellets are largely governed by the form and degree of bonding achieved between ore particles and the stability of these bonding phases during reduction of iron oxides ( Panigraphy et al., 1990 ). ⁎ Corresponding author at: R&D, Tata Steel Ltd, Burma mines post, Jamshedpur, 831007, Jharkhand, India. Tel.: +91 6572148928 (Of fi ce), +91 9204058889 (mobile); fax: +91 65722717. E-mail address: srinivasd@tatasteel.com (S. Dwarapudi). 0301-7516/$ – see front matter © 2011 Elsevier B.V. All rights reserved. doi: 10.1016/j.minpro.2011.03.004 In fl uxed pellets, the bonding is achieved through silicate melt formation during induration. The amount of gangue in the concen- trate, CaO & MgO in the fl uxes and binder in fl uences the amount and chemistry of silicate melt. CaO fl uxes silicate melt as well as reacts with iron oxide to form different calcium ferrites. MgO either enters the magnetite lattice to form magnesioferrite or dissolves in the slag phase. These melting phases interact with each other and dissolve a variable amount of iron oxides. As the formation of phases and microstructure during induration depends on the type and amount of fl uxes added, there is a need to study the effect of these fl uxing agents in terms of CaO/SiO ratio and MgO content on pellet quality. Wynnyckyj et al. presented results of adding CaO in the form of lime on fi red pellet quality; they found addition of lime increases the pellet shrinkage and hence increase the pellet strength due to the formation of calcium silicate and calcium ferrites ( Wynnyckyj and Fahidy, 1974 ). Hamilton et al. revealed that CaO fl uxed pellets exhibit improved strength when fi red between 1200 °C and 1400 °C due to the formation of more slag in the porous structures and consolidation of the pellet. ( Hamilton, 1976 ). Panigraphy, S.C et al. presented detailed results of limestone and dolomite fl uxed pellets from hematite concentrate; in limestone fl uxed pellets silicate melt was the predominant bonding phase up to " id="pdf-obj-0-17" src="pdf-obj-0-17.jpg">

Effect of pellet basicity and MgO content on the quality and microstructure of hematite pellets

Srinivas Dwarapudi a , , Tamal K. Ghosh a , Amitabh Shankar a , Vilas Tathavadkar a , D. Bhattacharjee a , R. Venugopal b

a R&D, Tata Steel Ltd, Jamshedpur, India b FME, ISM University, Dhanbad, India

article info

Article history:

Received 18 September 2010 Received in revised form 24 March 2011 Accepted 27 March 2011 Available online 1 April 2011

Keywords:

Pellet induration Swelling Acid pellets Reduction degradation index Silicate melt MgO pellets

abstract

Quality of pellets is inuenced by the nature of ore or concentrate, associated gangue, type and amount of uxes added and their subsequent treatment to produce pellets. These factors in turn result in the variation of physicochemical properties of the coexisting phases and their distribution during pellet induration. In the present study, effect of pellet basicity and MgO content on the melt formation and microstructure during the

induration was examined. Fired pellets with varying basicity (0 to 0.8) and MgO (0 and 1.5%) content were

tested for cold strength, reduction degradation index, reducibility, swelling and softeningmelting characteristics. Optical microscope studies with image analysis software were carried out to estimate the amount of different phases. SEM-EDS analysis was done to record the chemical analysis of oxide and slag phases. X-ray mapping was also carried out to understand the distribution of CaO, MgO, SiO 2 and Al 2 O 3 in different phases. From the results, it was observed that with increasing basicity, RDI and softeningmelting characteristics of pellets found to be improved. Addition of MgO to both acid and limestone uxed pellets considerably reduced their swelling tendency. Improved pellet quality could be attributed to the formation of sufcient amount of silicate melt in basic pellets and high melting point slag in MgO pellets. Limestone uxed pellets at 0.8 basicity, pyroxenite uxed pellets at 1.5% MgO and dolomite uxed pellets at 0.4 basicity & 1.5% MgO exhibited optimum metallurgical properties among all the pellets studied. © 2011 Elsevier B.V. All rights reserved.

1. Introduction

Iron ore agglomerate quality plays a vital role in decreasing the reducing agent consumption and increasing the productivity of blast furnace. In most of the integrated steel works, the burden mix for blast furnace is decided as per the availability of the iron ore agglomerates like sinter and pellets. More attention has been given in recent years to the use of uxed pellets in blast furnace due to their good strength and improved reducibility, swelling and softeningmelting charac- teristics. Generally, quality of pellets is inuenced by the nature of ore or concentrate, associated gangue, type and amount of uxes added and their subsequent treatment to produce pellets. These factors in turn result in the variation of physicochemical properties of the coexisting phases and their distribution during pellet induration. Hence properties of the pellets are largely governed by the form and degree of bonding achieved between ore particles and the stability of these bonding phases during reduction of iron oxides (Panigraphy et al., 1990).

Corresponding author at: R&D, Tata Steel Ltd, Burma mines post, Jamshedpur, 831007, Jharkhand, India. Tel.: +91 6572148928 (Ofce), +91 9204058889 (mobile); fax: +91 65722717. E-mail address: srinivasd@tatasteel.com (S. Dwarapudi).

0301-7516/$ see front matter © 2011 Elsevier B.V. All rights reserved.

In uxed pellets, the bonding is achieved through silicate melt formation during induration. The amount of gangue in the concen- trate, CaO & MgO in the uxes and binder inuences the amount and chemistry of silicate melt. CaO uxes silicate melt as well as reacts with iron oxide to form different calcium ferrites. MgO either enters the magnetite lattice to form magnesioferrite or dissolves in the slag phase. These melting phases interact with each other and dissolve a variable amount of iron oxides. As the formation of phases and microstructure during induration depends on the type and amount of uxes added, there is a need to study the effect of these uxing agents in terms of CaO/SiO 2 ratio and MgO content on pellet quality. Wynnyckyj et al. presented results of adding CaO in the form of lime on red pellet quality; they found addition of lime increases the pellet shrinkage and hence increase the pellet strength due to the formation of calcium silicate and calcium ferrites (Wynnyckyj and Fahidy, 1974). Hamilton et al. revealed that CaO uxed pellets exhibit improved strength when red between 1200 °C and 1400 °C due to the formation of more slag in the porous structures and consolidation of the pellet. (Hamilton, 1976). Panigraphy, S.C et al. presented detailed results of limestone and dolomite uxed pellets from hematite concentrate; in limestone uxed pellets silicate melt was the predominant bonding phase up to

  • 44 S. Dwarapudi et al. / International Journal of Mineral Processing 99 (2011) 4353

the basicity of 1.3. With increasing basicity more amount of liquid phase was formed during induration and hence more strength and less porosity. It was noted that the reducibility reaches a maximum at basicity 1.3 and then decreases with increased basicity. In low basicity pellets, during reduction of wüstite, a dense iron layer forms around slowing down the reduction, whereas at 1.3 basicity, relatively small grain size of hematite before reduction provides large surface area for reduction. Reducibility decreased beyond 1.3 basicity due to the formation of large secondary hematite grains. In limestone uxed pellets, swelling found to be highest at 0.8 basicity and decreased thereafter due to the formation of stronger bonding phase that can absorb hematite to magnetite transformation stress. It was also reported that dolomite uxed pellets exhibited higher porosity in comparison to limestone pellets, as MgO, being a major constituent of dolomite, raises the liquidus temperature of slag. Strength of dolomite pellets was found to be lower due to the high amount of porosity. Dolomite addition also improved the reducibility, highest at 1.3 basicity (Panigraphy et al., 1990). John J Friel et al. studied effect of dolomite addition on the magnetite pellets; pellets with basicity up to 1.3 exhibited less low temperature disintegration, whereas at basicity more than 0.8 exhibited less swelling. Pellets containing 1.5% MgO showed highest reduction characteristics and improved softening characteristics (Frill and Erickson, 1980). Sugiyama et al. studied the effect of CaO/SiO 2 and MgO/SiO 2 ratio on the pellet quality; MgO addition, in the form of magnesite, resulted in the formation of magnesioferrite and with increasing MgO porosity and reducibility increased and swelling decreased. Pellets without any CaO and MgO/SiO 2 ratio more than 0.6 exhibited improved reduc- ibility and softening properties, as the MgO increases the melting point of slag (Sugiyama et al., 1983). Earlier work reported by authors itself, revealed the MgO addition in the form of pyroxenite reduced the swelling substantially due to the formation of low FeO slag that can resist reduction stresses (Dwarapudi et al., 2010). Frazer et al. reported the effect of pellet basicity on swelling; high swelling observed in the basicity range of 0.20.8 was caused by the plasticnature of the slag which provides a medium for absorption of the reduction stresses by increased distances between the particles (Frazer et al., 1975). Yadav et al. established the inuence of MgO on sinter quality. It was reported that addition of MgO reduces the sinter strength by forming glassy dicalcium silicate suppressing calcium ferrite forma- tion. MgO restricts the melt formation during sintering, resulting in increased porosity, thereby increasing its reducibility and reduction degradation. MgO also improves the softeningmelting characteristics (Yadav et al., 2002). Bentell et al. reported the effect of MgO/SiO 2 ratio and CaO/SiO 2 ratio on pellet quality made from magnetite concentrate. Higher MgO/ SiO 2 ratio resulted in high porosity and low pellet strength. At higher CaO/SiO 2 ratio (in the range of 1.62.0), low temperature breakdown, reduction degree and strength of reduction of pellets found to be

improved. CaO/SiO 2 ratio beyond 2.0 is not favored due to the formation of 2CaOSiO 2 . They also reported that high temperature reducibility increases with MgO/SiO 2 ratio due to increase in the melting point of the binding phase (Bentell, 1981; Bentell et al., 1984). Lingtan K., et al. reported that addition of MgO in the form of olivine to pellets caused more low temperature breakdown due to the formation of cracks between the reduced magnetite phase and magnesioferrite spinel. However MgO improved the high temperature reducibility of pellets due to less liquid slag formation (Lingtan et al., 1983). It is important to note that conditions and parameters of pelletizing are specic to given ore or concentrate; the present study is undertaken for typical Indian hematite ore nes high in alumina. Except authors earlier work on quality of pellets from Indian iron ore (Dwarapudi et al., 2008, 2010; Dwarapudi and Ranjan, 2010), there is no considerable literature reported on the effect of pellet basicity and MgO content in the basicity range of 0 to 0.8 for Indian hematite ore. In the present study, pellets with varying basicity and MgO content were tested for cold strength, reduction degradation index, reducibility, swelling and softeningmelting characteristics. Optical microscope studies with image analysis software were carried out to estimate the amount of different phases. SEM-EDS analysis was done to record the chemical analysis of oxide and slag phases. X-ray mapping was also carried out to understand the distribution of CaO, MgO, SiO 2 and Al 2 O 3 in different phases. It was attempted to establish correlation between pellet chemistry (in terms of basicity & MgO) and quality.

2. Experimental

The following materials were used for preparing the green pellets:

iron ore nes (10 mm size); bentonite (75 microns); anthracite coal (10 mm); limestone (50 mm), dolomite (50 mm) and pyroxenite (50 mm). Iron ore nes, coal, limestone, dolomite and pyroxenite were ground separately in laboratory ball mill to get the required neness for pelletizing. The chemistry and neness of the all the materials used are mentioned in author's earlier work related to pyroxenite ux usage. (Dwarapudi et al., 2010). Pyroxenite is a magnesium silicate rock composed largely of pyroxene with small amounts of olivine and serpentine. Green pellets were prepared using a laboratory balling disc with a diameter of 600 mm, an edge height of 200 mm and a tilting angle of 45° at 27 rpm. During balling, green pellets were screened with 10 mm and 12.5 mm screens to get 1012.5 mm pellets. The amount of ingredients added for preparing green pellets with varying basicity and MgO (Pellet A,A1, B,B1, C,C1, D,D1, E &E1) and their quality parameters are shown in Table 1. To adjust the basicity of pellets from 0 to 0.8, amount of limestone was varied from 0 to 3% in the green pellets. To study the effect of MgO content on the uxed pellet quality, pellets were prepared in the basicity range of 0 to 0.8 with 1.5% MgO. The reason behind selection 1.5% MgO was mentioned elsewhere by the author in their earlier work (Dwarapudi et al., 2010). To adjust the MgO content, dolomite dosage was varied from 2 to 6% and pyroxenite

Table 1 Ingredients of green pellets with varying amount of uxes and their quality.

 

Pellet A

Pellet A1

Pellet B

Pellet B1

Pellet C

Pellet C1

Pellet D

Pellet D1

Pellet E

Pellet E1

Iron ore, wt.%

97.8

93.3

97.3

92.8

96.6

92.5

95.9

92.1

95.1

91.7

Bentonite, wt.%

0.8

0.7

0.8

0.7

0.8

0.7

0.8

0.7

0.8

0.7

Limestone, wt.%

0.0

0.0

0.5

0.0

1.3

0.0

2.0

0.0

2.8

0.0

Dolomite, wt.%

0.0

0.0

0.0

2.0

0.0

3.5

0.0

4.7

0.0

5.6

Pyroxenite, wt.%

0.0

4.7

0.0

3.2

0.0

1.9

0.0

1.2

0.0

0.6

Coal, wt.%

1.4

1.3

1.4

1.3

1.4

1.3

1.3

1.3

1.3

1.3

Green pellet quality Drop number

4.6

4.3

3.9

2.7

3.7

2.8

4.3

3.7

4.4

4.5

Green crushing strength, kg/pellet

1.6

1.7

1.8

1.9

1.8

1.9

1.9

1.9

1.8

2.0

Green pellet moisture,%

7.9

7.9

7.6

7.1

7.4

7.3

6.9

7.2

7.6

7.1

S. Dwarapudi et al. / International Journal of Mineral Processing 99 (2011) 4353

Table 2

Chemical analysis of pellets with varying basicity and MgO content.

45

wt.%

Pellet A

Pellet A1

Pellet B

Pellet B1

Pellet C

Pellet C1

Pellet D

Pellet D1

Pellet E

PelletE1

Fe(t)

SiO 2

Al 2 O 3 CaO

MgO

CaO/SiO 2

66.0

1.9

2.2

0.1

0.1

0.0

63.6

4.2

2.0

0.1

1.5

0.0

65.8

2.0

2.1

0.5

0.2

0.2

63.2

3.6

2.1

0.9

1.6

0.3

65.4

1.9

2.2

0.8

0.2

0.4

64.0

2.9

2.1

1.3

1.5

0.4

65.0

2.2

2.1

1.4

0.3

0.6

63.7

2.7

2.2

1.7

1.7

0.6

64.8

1.9

2.2

1.6

0.2

0.8

63.2

2.5

2.1

2.0

1.7

0.8

addition from 0.5 to 3%. Before ring, pellets were dried in the hot air oven at 150 °C for 56 h to ensure that all the moisture is removed. Firing of the pellets was carried out using electrically heated rotary hearth furnace (RHF) mentioned elsewhere by the author in their earlier work (Dwarapudi et al., 2010). The RHF consists of 5 heating zones and 1 cooling zone. All the zones were provided with air inlet nozzles to inject ambient air for creating oxidizing atmosphere during induration. During ring, air was injected from zone-6 (cooling zone) and was vented from the exhaust hood in zone 1 to ensure hot air

circulation from zone 6 to zone 1 while pellet sample travels from zone 1 to zone 6. The countercurrent movement between the hot pellets and air facilitates the complete oxidation of admixed coal in the green pellets. Temperature proles in each zone were maintained to simulate the ring conditions in the industrial pellet indurating machine. Temperature in zone-1 & 2 was maintained at 800 °C & 1100 °C respectively to simulate preheating, zone-3 & 4 at 1300 °C to simulate ring and zone-5 & 6 at 1100 °C & 800 °C respectively to simulate cooling zones of indurating machine. Inconel baskets, that

(a) Pellet A (b) Pellet B (c) Pellet C (d) Pellet D (e) Pellet E
(a) Pellet A
(b) Pellet B
(c) Pellet C
(d) Pellet D
(e) Pellet E

Fig. 1. Optical microstructures of red MgO-free pellets with varying basicity.

  • 46 S. Dwarapudi et al. / International Journal of Mineral Processing 99 (2011) 4353

can accommodate 500 g of pellets, were used to re the pellets in the RHF. In each batch 3 kg of pellets were red to generate required number samples for the test work. Table 2 shows the chemical analysis of red pellets with varying basicity and MgO content.

  • 2.1. Physical and metallurgical testing of pellets

Fired pellets were tested for their cold compression strength (CCS) as per ISO 4700 and swelling index as per ISO4698. While reporting CCS, standard deviation was also measured. Reduction degradation index (RDI) and reducibility index (RI) were tested as per ISO 4696-2 and ISO 7215 respectively. For swelling, reducibility and reduction degradation index, average of two test readings was taken and error bars are added to the graphs with 90% condence level. For softeningmelting test, mixed burden sample of 280 g is prepared using sinter (154 g), pellets (98 g) and lump ore (28 g) in the ratio of 35%, 55% and 10%. Schematic diagram of apparatus used for softeningmelting test with the description of test procedure was mentioned elsewhere by the author in their earlier work (Dwarapudi et al., 2010). For micro structural studies, CCS and swelling, pellets from each batch were collected from top layer of Inconel basket as they are exposed to uniform heat from top and sidewalls of RHF. Pellets with cracks and irregular shape were avoided as they experience uneven heat treatment across their cross section.

  • 2.2. Image analysis of microstructures

Image analysis is a technique that is used to provide an objective measurement of different phases in microstructure. Pellet samples were cut into half and hot mounted at 175 °C temperature and 90 daN load for 14 min using a conductive resin. Once sample has been mounted and polished, it was placed under the Zeiss-Axioplan2 microscope for examination. A black and white CCD digital camera with a maximum resolution of 756 × 581 pixels was mounted behind the lens of the microscope to capture the light reected from the sample. A 10× eye piece and 20× objective lens on the microscope has been selected for the current study. At this level of magnication, the view frame on the sample surface is approximately 0.7 × 0.5 mm. The signal from the camera was provided to a personal computer through a gain correction amplier to correct the signal for optimal display. The computer software used for interpreting the camera signal into digital image was Axiovision 4.7 Imaging Systemsupplied by Carl Zeiss Vision. Basically, the digital image captured from the black and white camera is represented by pixels having 256 shades of grey values i.e. 0 to 255 (Loo and Leung, 2003). The lower range of grey values represents pores and the oxide grains represent higher range values. A digitized black and white photograph was transformed into a segmented image with the specied range of grey values to different phases. Once the image has been processed, image analysis tools from the Axiovision software were used to measure the area fraction and phase density of different phases in the microstructure.

3. Results

  • 3.1. Quantitative measures of microstructure through image analysis

3.1.1. Pellets with varying basicity (referred as MgO-free pellets) Fig. 1 shows the optical microstructures of red pellets with varying basicity. Image analysis studies of these pellets revealed that hematite, magnetite and silicate melt are the major phases in the pellets. Amount of silicate melt, which acts as a bonding phase, was found to increase with increasing basicity, as shown in Fig. 2(a). Distribution of silicate melt is measured in terms of silicate melt density (number of silicate melt phases per unit area) using image analysis technique as shown in Fig. 2(b). If the silicate melt is more

46 S. Dwarapudi et al. / International Journal of Mineral Processing 99 (2011) 43 – 53

Fig. 2. Image analysis of MgO-free pellets (a) Distribution of different phases and (b) silicate melt density.

distributed, there will be more number of phases/grains per unit area, i.e. high silicate melt density. The distribution of the silicate melt phase is more scattered in 0.4 and 0.6 basicity pellets, as indicated by high silicate melt density. This could be attributed to the increased mobility of the melt phase due to the formation of low melting point olivines in this basicity range (Frazer et al., 1975). Porosity found to decrease with increasing basicity due to impregnation of pores with the melt phase.

3.1.2. Pellets with varying basicity with 1.5% MgO (referred as MgO pellets) Fig. 3 shows the optical microstructures of red MgO pellets (with varying basicity at 1.5% MgO). Image analysis studies, as shown in Fig. 4(a) of these pellets revealed that hematite, magnetite and silicate melt are the major phases, while some amount of magnesioferrite was observed at low basicity levels. The mean size of the pores was found to increase with increasing basicity as indicated by low pore density, Fig. 4(b). Pore density (no of pores/mm 2 ) is an indication of pore size. Higher the pore density more the number of pores in a given area with small pore size and vice versa.

3.2. SEM study with EDS analysis

3.2.1. MgO-free pellets Fig. 5 shows the SEM image of Pellet A, C & E with EDS analysis of all pellets (A, B C, D & E). From the results it was evident that chemistry of iron oxides is uniform in all pellets irrespective of basicity. But chemistry of slag phase found to be varying with increasing basicity. FeO content of the slag phase decreased considerably with increased basicity as shown in the EDS analysis of

S. Dwarapudi et al. / International Journal of Mineral Processing 99 (2011) 4353

47

(a)Pellet A1 (b)Pellet B1 (c)Pellet C1 (d)Pellet D1 (e)Pellet E1
(a)Pellet A1
(b)Pellet B1
(c)Pellet C1
(d)Pellet D1
(e)Pellet E1

Fig. 3. Optical microstructures of red MgO pellets with varying basicity.

Fig. 5. X-ray mapping studies of the red pellet samples, as shown in Fig. 6, revealed that CaO from the limestone was distributed only in silicate melt.

3.2.2. MgO pellets

Fig. 7 shows the SEM image of Pellet A1, C1 & E1 with EDS analysis of all pellets (A1, B1 C1, D1 & E1). Addition of MgO to varying basicity pellets increased the FeO content of the slag phase as shown in the EDS analysis. X-ray mapping studies of the red MgO pellet samples, as shown in Fig. 8, revealed that MgO was distributed both in silicate melt and oxide phase.

3.3. Cold compression strength

Cold compression strength (CCS) indicates the ability of pellets to withstand the load during their storage & handling and the load of burden material in the reduction furnace. Blast furnace needs pellets with CCS values in the range of 200230 kg/pellet. Pellet strength

found to increase up to 0.4 basicity (CaO/SiO 2 ) in MgO-free pellets and decreased thereafter. The same trend was observed in MgO pellets also. But MgO pellets exhibited slightly lower strength compared to basic pellets as shown in Fig. 9. Both the pellets, MgO-free and MgO, exhibited required strength values as desired by the blast furnace.

3.4. Swelling index

Swelling index indicates volume change of pellets during reduction. Higher swelling index reduces the strength of pellets after their reduction thereby causing irregularities in the blast furnace like high resistance to gas ow, burden hanging and slipping. Maximum allowable swelling of pellets for blast furnace ranges from 14 to 16%. Fig. 10 shows the swelling index of MgO-free and MgO pellets with varying basicity. Error bars are shown in the gure with 90% condence level of the test results. From the results it is evident that acid pellets (zero basicity and no MgO content) exhibited highest swelling among all the pellets. In case of MgO-free pellets, high

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48 S. Dwarapudi et al. / International Journal of Mineral Processing 99 (2011) 43 – 53

Fig. 4. Image analysis of red MgO pellets with varying basicity (a) Distribution of different phases and (b) pore density.

swelling was observed at 0.6 basicity and decreased thereafter. MgO pellets demonstrated considerably lower swelling tendency com- pared to MgO-free pellets at all basicity levels.

  • 3.5. Reduction degradation and reducibility

Reduction degradation index (RDI) of pellets indicates their tendency to generate nes during reduction. From the results it is evident that acid pellets exhibited highest RDI whereas MgO-free pellets in the basicity range of 0.20.8 showed low RDI as shown in Fig. 11. MgO pellets demonstrated lower RDI compared to MgO-free pellets in the basicity range of 0 to 0.4, but high RDI in 0.60.8 basicity range. Reducibility of the pellets may be dened as the ease with which the oxygen combined with the iron oxide can be removed. A higher reducibility indicates more indirect reduction in the blast furnace resulting in lower coke rate and high productivity. Results indicated that acid pellets reduced more compared to MgO-free pellets whereas MgO pellets exhibited higher reducibility compared to acid and MgO- free pellets irrespective of their basicity as shown in Fig. 12.

  • 3.6. Softeningmelting characteristics

Study of softeningmelting characteristics of pellets help in understanding the formation of cohesive zone in the lower portion of blast furnace. If the pellets soften at lower temperature and the temperature range between softening and melting is wider, then the resistance to the gas ow will be more in the cohesive zone. Results indicated that softening temperature of MgO-free pellets increased with increasing basicity and the softeningmelting range decreased

considerably, Fig. 13. MgO pellets showed increased softening temperature and decreased softeningmelting range at 0.4 basicity only as shown in Fig. 14.

4. Discussion

  • 4.1. Pellet strength

Fig. 9 above mentioned showed that CCS of both MgO-free pellets and MgO pellets are above the acceptable limit for blast furnace. Highest strength of MgO-free pellets at 0.4 basicity could be attributed to decreased porosity with increased basicity. Addition of basic ux resulted in the formation of more amount of low strength silicate melt phase, Fig. 2(a). Silicate melt lls up the pores between solid particles and exerts pressure to pull them together due to interfacial forces thereby reducing the porosity. But beyond 0.4 basicity, the positive effect of low porosity is counteracted by the increased amount of low strength silicate melt, thereby resulting in lower strength. Strength of MgO pellets found to be lower as compared to MgO- free pellets irrespective of basicity. This could be attributed to high amount of silicate melt, Fig. 4 (a), which is low in strength, in MgO pellets compared to MgO-free pellets.

  • 4.2. Swelling behavior

Volumetric expansion of iron ore pellets takes place during their reduction from hematite to magnetite and wüstite. It can be mainly attributed to the increased volume requirements for the anisotropic growth of magnetite (111) planes parallel to the hematite (0001) planes (Frazer et al., 1975). Swelling is related to the ability of gangue or slag phase to withstand the reduction stresses of independent oxide particles. High melting point slag would produce sufcient bonding strength to limit swelling and low melting point slag enhances swelling. As shown in Fig. 10, acid pellets (0 basicity and 0% MgO content) exhibited highest swelling and MgO-free pellets exhibited higher swelling at 0.6 basicity and decreased thereafter. In acid pellets reduction is accompanied by the reaction between Fe 2+ and SiO 2 to form low melting point phase, fayalite (Fe 2 SiO 4 ) that melts at 1175 °C (Dwarapudi et al., 2010). High swelling index of these pellets can be attributed to the plastic or mobile nature of low melting point fayalitic slag that provides a medium for absorption of the reduction stresses by increased distances between the particles. In MgO-free pellets, high swelling values at 0.6 basicity can be compared to the earlier studies of Frazer et al. on different iron ore nes. They reported that maximum swelling on reduction occurs in the basicity range of 0.20.8. In case of our pellets, maximum swelling at 0.6 basicity can be attributed to the formation of low melting point calcium olivines between Fe 2 SiO 2 and Ca 2 SiO 4 , with lowest melting point of 1115 °C (Frazer et al., 1975). High silicate melt density of 0.40.6 basicity pellets as shown in Fig. 2(b), also conrms the plastic or mobile nature of the low melting point slag. Addition of MgO to pellets increases the melting point of the slag or silicate melt formed between the oxide particles (Onoda et al., 1980). Low swelling of MgO pellets, Fig. 10, can be attributed high melting point slag that contributes sufcient bond strength to withstand the reduction stresses.

  • 4.3. Reduction degradation and reducibility

Reduction degradation (measured as RDI) of pellets is an undesired phenomenon that occurs at low temperatures in the upper part of blast furnace or reduction shaft of any direct reduction unit. The primary cause of low temperature disintegration is due to crystalline transformation from hexagonal hematite to cubic magne- tite accompanied by volume expansion to an extent of 25% and lattice distortion (Panigraphy et al., 1984). The anisotropic dimensional change due to the transformation leads to severe stresses in certain

S. Dwarapudi et al. / International Journal of Mineral Processing 99 (2011) 4353

49

S. Dwarapudi et al. / International Journal of Mineral Processing 99 (2011) 43 – 53 49

Fig. 5. SEM image of Pellet A, C & E with EDS analysis of all pellets (A, B, C, D & E).

S. Dwarapudi et al. / International Journal of Mineral Processing 99 (2011) 43 – 53 49

Fig. 6. Distribution of Fe, Si, Ca and Mg in red MgO-free pellet with 0.8 basicity (Pellet E).

  • 50 S. Dwarapudi et al. / International Journal of Mineral Processing 99 (2011) 4353

50 S. Dwarapudi et al. / International Journal of Mineral Processing 99 (2011) 43 – 53

Fig. 7. SEM image of Pellet A1, C1 & E1 with EDS analysis of all pellets (A1, B1, C1, D1 & E1).

50 S. Dwarapudi et al. / International Journal of Mineral Processing 99 (2011) 43 – 53

Fig. 8. Distribution of Fe, Si, Ca and Mg in red MgO pellet with 0.4 basicity (Pellet D1).

S. Dwarapudi et al. / International Journal of Mineral Processing 99 (2011) 4353

290 50 270 45 250 40 230 35 0%MgO 1.5%MgO 210 30 Stdev 0%MgO Stdev 1.5%MgO
290
50
270
45
250
40
230
35
0%MgO
1.5%MgO
210
30
Stdev 0%MgO
Stdev 1.5%MgO
190
25
170
20
150
15
0
0.2
0.4
0.6
0.8
Cold copression strength, kg/pellet
Standard deviation
50 45 40 0%MgO 35 1.5%MgO 30 25 20 15 10 5 0 0 0.2 0.4
50
45
40
0%MgO
35
1.5%MgO
30
25
20
15
10
5
0
0
0.2
0.4
0.6
0.8
RDI,% (-3.15mm)

Pellet basicity

Fig. 11. Effect of pellet basicity on the RDI of red pellets.

51

Fig. 9. Effect of pellet basicity on the cold strength of red pellets.

planes, resulting cracks in brittle matrix. The effect is particularly severe in the grain boundaries. It is very clear that iron oxide in the indurated pellets is mainly in the form of hematite; therefore, generation of internal stress in principle is unavoidable. The disintegration can be reduced by increasing the amount of stable bonding phases, which are less brittle at lower temperatures, with homogeneous distribution. Bonding which forms during induration can be divided into three main groups: iron oxides bonds (hematite, magnetite), silicate bonds and local bonds (calcium ferrite, magne- sioferrite) that are close to particular mineral phases. Iron oxide bonds are common and strong, but they are not stable during reduction due to their phase change. Unlike iron oxide bonds, silicate bonds remain unaltered during reduction and they soften and melt later (Niiniskorpi, 2004). Acid pellets showed high reduction degradation due to the presence of more hematite bonds and less silicate bonds. MgO-free pellets exhibited considerably less reduction degradation due to the presence of silicate melt, as shown in Fig. 2(a), which is more stable compared to hematite. In the earlier studies by the author, it was observed that uniformly distributed silicate melt improves the RDI of iron ore pellets (Dwarapudi et al., 2008). MgO pellets exhibited less degradation compared to MgO-free pellets up to 0.4 basicity. This could be attributed to the comparatively high amount of silicate melt as shown in Fig. 4(a). But the poor degradation of MgO pellets in the basicity range of 0.6 to 0.8 could be attributed to the increased pore size, as indicated by low pore density, Fig. 4(b), which can result in poor strength of reduced pellet matrix and hence more degradation. Pore density (no of pores/mm 2 ) is an indication of pore size. Higher the pore density more the number of pores in a given area with small pore size and vice versa.

50 45 40 0% MgO 35 1.5% MgO 30 25 20 15 10 5 0 0
50
45
40
0% MgO
35
1.5% MgO
30
25
20
15
10
5
0
0
0.2
0.4
0.6
0.8
Swelling Index,%

Pellet basicity

Fig. 10. Effect of pellet basicity on the swelling of red pellets.

As shown in Fig. 12, reducibility of acid pellets is higher than MgO- free pellets due to the presence of more amount of low melting point silicate melt between the iron oxide grains in the later. During reduction at high temperature, the slag softens and impedes the ow of reducing gas within the pellet thereby retarding the reduction. In case of MgO pellets, silicate melt formed between the iron oxide gains is high in melting point (Onoda et al., 1980) due to MgO. Relatively high reducibility of these pellets at all basicity levels can be attributed to high melting point slag which does not soften at reduction temperatures and keeps the pores open for reducing gas thereby enhancing reduction.

4.4. Softeningmelting characteristics

Softeningmelting properties of the pellets are affected by the liquidus phase with low melting point that is formed between wüstite and slag phase during reduction (Onoda et al., 1980). Inferior softeningmelting characteristics of acid pellets can be attributed to the FeO rich low melting fayalitic liquidus slag, whereas MgO-free pellets exhibited superior properties due to the fact that increase in pellet basicity increases the basicity of burden (55% Sinter+ 35% pellets+ 10%lump ore) slag thereby increasing its liquidus temper- ature as given in Table 3. Burden slag consists of slag formed from all the iron burden, viz., sinter, pellets and lump ore. Increased basicity of burden slag facilitates the formation of discacium silicate, which has narrow melting range, thereby decreasing the softeningmelting range as shown in Fig. 13. MgO pellets exhibited high softening temperature and low SM range at 0.4 basicity as shown in Fig. 14. This could be due to the formation of optimum slag similar to the slag formed by MgO-free pellets at 0.8 basicity. Four component basicity (CaO+MgO/(SiO 2 + Al 2 O 3 ) and viscosity of both the slags are similar as shown in Table 3,

that means slag with optimum liquidus temperature and viscosity is

90 85 80 75 70 65 0%MgO 1.5%MgO 60 55 50 0 0.2 0.4 0.6 0.8
90
85
80
75
70
65
0%MgO
1.5%MgO
60
55
50
0
0.2
0.4
0.6
0.8
Reducibility Index, %

Pellet basicity

Fig. 12. Effect of pellet basicity on the reducibility of red pellets.

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52 S. Dwarapudi et al. / International Journal of Mineral Processing 99 (2011) 43 – 53

Fig. 13. Effect of pellet basicity on the softeningmelting characteristics of mixed burden.

52 S. Dwarapudi et al. / International Journal of Mineral Processing 99 (2011) 43 – 53

Fig. 14. Effect of pellet basicity at 1.5% MgO on the softeningmelting characteristics of mixed burden.

required for optimum softeningmelting characteristics. Calculation method of viscosity is mentioned elsewhere by one of the authors (Shankar et al., 2007). Low amount of non-drip material in case of MgO-free pellets at 0.8 basicity and MgO pellet at 0.4 basicity also indicates that burden slag formed is easily owable without impeding the burden permeability. After evaluating the pellets for different metallurgical properties, it is often difcult to directly ascertain the optimum pellet chemistry suitable for blast furnace because some quality parameters like reducibility, degree of reduction need to be maximized where as other

52 S. Dwarapudi et al. / International Journal of Mineral Processing 99 (2011) 43 – 53

Fig. 15. Composite quality index of varying basicity pellets with and without MgO.

parameters like swelling and softeningmelting range need to be minimized. To calculate the numerically optimum pellet chemistry, a new dimensionless index called composite quality indexhas been formulated. Similar attempts were made earlier by other workers to formulate integral index for green pellets (Zhak et al., 1998) and integral indices for metallurgical conversions (Yusn et al., 1997). Composite quality index (CQI) is composed of different indices related to high temperature metallurgical properties of pellets. Indices that need to be increased viz., reducibility index and degree of reduction are placed in the numerator whereas indices that need to be decreased, viz., reduction degradation index, swelling index and softeningmelting range are place in the denominator. Hence higher composite index indicates the improved pellet quality and vice verse. Composite quality index (CQI)= (reducibility index+ degree of reduction)/(reduction degradation index+ swelling index+ SM range). Fig. 15 shows the CQI of MgO-free and MgO pellets. In MgO- free pellets highest CQI value (0.74) is observed at 0.8 basicity. Pyroxenite uxed pellets (zero basicity and 1.5% MgO) and dolomite uxed pellets (0.4 basicity and 1.5% MgO) also exhibited high CQI values, 0.58 and 0.59 respectively. The CQI, which gives weightage to vital quality parameters, can be used as a tool to relatively compare the pellet quality rather relying on any single parameter.

5. Conclusions

The effect of pellet basicity and MgO content on the melt formation and microstructure during the induration of iron ore pellets was examined. Fired pellets with varying basicity (0 to 0.8) and MgO (0 and 1.5%) content were tested for cold strength, reduction degradation index, reducibility, swelling and softeningmelting characteristics.

Table 3 Details of burden sample and slag chemistry from softeningmelting test.

 

Pellet A

Pellet B

Pellet C

Pellet D

Pellet E

Pellet A1

Pellet B1

Pellet C1

Pellet D1

PelletE1

Mixed burden sample used for SM test wt. of sinter, g

154.0

154.0

154.0

154.0

154.0

154.0

154.0

154.0

154.0

154.0

wt. of pellets, g

98.1

98.1

98.1

98.1

98.1

98.1

98.1

98.1

98.1

98.1

wt. of ore, g

28.0

28.0

28.0

28.0

28.0

28.0

28.0

28.0

28.0

28.0

Burden slag chemistry after softeningmelting test CaO, wt.%

44.2

44.5

45.2

45.4

46.5

40.3

40.9

43.3

43.7

43.7

SiO 2 ,wt.%

28.6

28.6

27.7

28.2

27.1

31.9

29.6

28.4

27.7

25.8

MgO, wt.%

7.3

7.9

7.7

8.1

7.6

10.8

12.8

10.9

11.4

13.6

Al 2 O 3 , wt.%

19.9

19.1

19.2

18.2

18.6

16.9

16.6

17.5

17.3

16.8

Slag weight, g

31.6

32.4

32.7

33.9

33.2

34.9

36.6

35.3

36.0

36.5

CaO/SiO 2

1.5

1.6

1.6

1.6

1.7

1.3

1.4

1.5

1.6

1.7

(CaO+MgO)/(SiO 2 +Al 2 O 3 )

1.01

1.1

1.1

1.2

1.2

1.1

1.2

1.2

1.2

1.3

Calculated liquidus temperature of slag, °C

1426

1436

1466

1466

1496

1436

1461

1466

1476

1476

Non drip material, %

17.3

21.5

11.9

17.3

8

14.2

19.4

2.8

11.3

15.4

Calculated slag viscosity (poise)

2.0

1.8

1.7

1.5

1.4

2.0

1.5

1.4

1.2

0.9

S. Dwarapudi et al. / International Journal of Mineral Processing 99 (2011) 4353

53

Optical microscope studies with image analysis software were carried out to estimate the amount of different phases. SEM-EDS analysis was done to record the chemical analysis of oxide and slag phases. X-ray mapping was also carried out to understand the distribution of CaO, MgO, SiO 2 and Al 2 O 3 in different phases. The following conclusions can be drawn from this work:

  • 1. With increasing basicity the amount of silicate melt, which acts a bonding phase, found to increase in the red pellets. FeO content of the silicate melt decreased with increasing basicity of pellets. Addition of MgO to both acid and limestone-uxed pellets resulted in the formation of high melting point slag during their induration.

  • 2. Acid pellets exhibited highest swelling, whereas maximum swelling in MgO-free pellets was observed at 0.6 basicity. Addition of MgO to both acid and limestone-uxed pellets at all basicity levels considerably reduced the swelling tendency of pellets due to the formation of high melting point slag that gives sufcient bond strength to withstand the reduction stresses.

  • 3. With increasing basicity, MgO-free and MgO pellets exhibited considerably lower reduction degradation compared to acid pellets due to the formation of more amount of silicate melt, which is more stable under the reducing conditions in blast furnace.

  • 4. Reducibility of MgO-free pellets is slightly lower compared to acid pellet due to the formation of silicate melt in the former which softens and impedes the ow of reducing gas within the pellet thereby retarding the reduction. Addition of MgO to both acid and limestone-uxed pellets at all basicity levels increased their reducibility by forming high melting point slag which does not soften at reduction temperatures and keeps the pores open for reducing gas thereby enhancing reduction.

  • 5. Inferior softeningmelting characteristics of acid pellets can be attributed to the formation of FeO rich low melting fayalitic liquidus slag. MgO-free pellets with increasing basicity exhibited increased softening temperatures and low softeningmelting range due to the formation of burden slag with high liquidus temperature.

  • 6. To relatively compare pellet quality based on vital quality parameters, a new dimensionless index called composite quality indexhas been formulated. Higher composite index indicates the improved pellet quality and vice verse. Limestone uxed MgO-free pellets at 0.8 basicity, pyroxenite uxed pellets at 1.5% MgO and dolomite uxed pellets at 0.4 basicity & 1.5% MgO exhibited optimum metallurgical quality parameters among all the pellets studied.

Acknowledgements

Authors are thankful Mr. Mark B Denys (Chief, R&D and SS) for his encouragement, support and permission to publish this paper. Thanks are also due to Prof A K Lahiri, Prof. T C Rao, Mr. Ashok Kumar (Chief, RMIMTG) and Mr. Surajit Sinha (Head Pellet plant) for their valuable inputs.

References

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