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Reduction swelling mechanism of hematite fluxed briquettes

  • Wang Ping , Wu Hao , Chun Tie-jun EMAIL logo , Zhou Song and Zhou Tian-bao
Published/Copyright: April 20, 2022
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High Temperature Materials and Processes
From the journal High Temperature Materials and Processes Volume 41 Issue 1

Abstract

The reduction swelling behaviors of the fluxed briquettes with basicity (CaO/SiO2) in the range of 0.33–1.33 were determined by adding analytical-grade CaO. Results showed that with the increase of basicity, the diameter, volume, and porosity of briquettes increased gradually, whereas the diameter, volume, and porosity of briquettes decreased when the basicity was greater than 0.83. The volume and porosity of briquettes decreased gradually with the increase in firing temperature. The reduction swelling index (RSI) reached the maximum at the basicity of 0.83. The RSI of fluxed briquettes was fired at 1,230°C, and that at the basicity of 0.83 was 20.12% after 60 min of reduction. The RSI of the fluxed briquettes was 3.16% when the basicity of briquettes was 0 upon firing at 1,300°C. The reducibility and swelling were positively correlated with internal porosity. The higher the swelling of briquettes, the denser was the distribution of iron whiskers. The lower the swelling of briquettes, the more closely the iron particles connected.

Keywords: fluxed briquettes; reduction swelling; porosity; iron whisker

1 Introduction

Theoretical and practical experience show that fine ore is suitable for sintering and the fine grinding concentrate is more suitable for pellets. China has a large number of domestic and imported iron concentrates. The production and usage of high-quality briquettes will increase as the technology of coal as fuel and briquette production continues to improve [1]. Considering the demand for energy saving, emission reduction, and the optimization of blast furnace charge structure, the proportion of briquettes in the furnace gradually increases and the basicity requirement of blast furnace slag cannot be met by using acid briquettes [2]. The swelling of the briquettes is a very important metallurgical property index in blast furnace smelting. The swelling behavior of briquettes has been extensively studied as early as the 1960s and 1970s, and many studies on the mechanism of swelling have been reported, however, conclusions on the production of iron whisker, the formation of low melting point slag, the induction of carbon deposition, and gas accumulation in pores during reduction were inconsistent [3,4,5,6,7,8,9,10,11,12,13,14,15]. In this study, the influence of basicity and firing temperature on the microstructure, reducibility, and reductive swelling properties of fluxed briquettes was determined and the mechanism of reducing swelling of fluxed briquettes was explained.

2 Raw materials and experimental methods

2.1 Raw materials

Analytical-grade reagents including Fe2O3, CaO, MgO, SiO2, and Al2O3 were used in this experiment. The starch was employed as the binder which could be decomposed during firing.

2.2 Experimental methods

Cylindrical briquettes with a diameter of 19 mm and height of 4 mm were produced by pressing a 3 g mixture of the raw materials and 1% starch solution with 0.5 wt% concentration into a cylindrical mold pressing at 20 MPa for 1 min. The chemical composition of briquettes is shown in Table 1, and the value of CaO content is based on the mixture values of SiO2, CaO, MgO, and Fe2O3.

Table 1

Chemical ratio of briquettes at different basicity values

Basicity (CaO/SiO2) CaO (%) SiO2 (%) MgO (%) Al2O3 (%) Fe2O3 (%)
0 0 3.0 0.5 0.5 96.0
0.33 1.0 3.0 0.5 0.5 96.0
0.67 2.0 3.0 0.5 0.5 96.0
0.83 2.5 3.0 0.5 0.5 96.0
1.0 3.0 3.0 0.5 0.5 96.0
1.33 4.0 3.0 0.5 0.5 96.0

The briquettes were dried at 105°C for 4 h in the oven. The dried briquettes were preheated at 950°C for 10 min and fired at 1,230, 1,250, 1,280, and 1,300°C for 20 min in a double-temperature zone horizontal tube furnace, and both ends of the tube were opened. After fired, the briquettes samples were mounted and polished, the microstructures of the samples were measured by scanning electron microscopy (SEM) with energy dispersive spectroscopy (EDS). The apparent and true densities of the fired briquettes were tested using a pycnometer and the tests were repeated thrice. The porosity (ε = 1 − ρ 1/ρ 2) of the fired briquettes was obtained using the apparent density (ρ 1) and true density (ρ 2).

Figure 1 shows a measuring device for reduction swelling index (RSI) and reducibility degree of briquettes. The specification of the reduction reactor is Φ 75 mm × 800 mm, and a 100 mm high alumina layer was placed at the bottom of the reactor. The high aluminum ball functions were used to preheat the reducing gas and stabilize the reducing gas flow. The briquettes were heated to 900°C under the protection of an N2 atmosphere of 0.83 L·min−1. The gas flow rate was 15 L·min−1 at 900°C (CO: N2 = 3:7) and kept for 60 min. After completing the reaction, the briquettes were cooled to 100°C under the protection of N2 (flow rate, 15 L·min−1).

Figure 1 Testing device for RSI and reducibility degree of briquettes.
Figure 1

Testing device for RSI and reducibility degree of briquettes.

The volume change of briquettes before and after the reduction reaction was measured using the water immersion method and the RSI of briquettes was calculated.

Equations (1) and (2) were used to calculate the reducibility degree and RSI of the fired briquettes as expressed below:

(1) Reducibility degree = [ ( m 0 − m 2 ) / ( m 0 × 0.430 × W 2 ) ] × 100 % ,

where m 0 and m 2 are the mass of briquette before and after reaction, respectively, in grams, and W 2 is the content of total Fe before reaction, %.

(2) RSI = [ ( V 1 − V 0 ) / V 0 ] × 100 % ,

where V 0 is the volume of the sample before the reduction in cm3 and V 1 is the volume of a sample after the reduction in cm3.

The reduced briquettes were observed by SEM with EDS to observe the morphology of the metallic iron on the briquette surface and analyze the chemical elements in the briquette. Therefore, we can explore the gangue composition for the reduction of swelling of hematite briquettes.

3 Results and discussion

3.1 Effect of basicity on the porosity of fired briquettes

Figure 2 shows the effect of basicity on the porosity of the fired briquettes. The porosity of the fired briquettes increased rapidly when the basicity was in the range of 0–0.83. The porosity of briquettes increased slowly or decreased slightly as the basicity of briquettes continued to increase (1.0–1.33). The porosity of briquettes with different basicity decreased gradually with the increase of firing temperature. The porosity of the briquettes, after firing, was 10.4% when the firing temperature was 1,230°C and the basicity of the briquettes was 0. The porosity of the briquettes after firing reached 24.11% when the basicity was 0.83. The porosity of fired briquettes with a basicity of 0 was only 5.12% at the firing temperature of 1,300°C.

Figure 2 Effect of basicity on the porosity of fired briquettes.
Figure 2

Effect of basicity on the porosity of fired briquettes.

Figure 3 shows the secondary electron image of briquettes with different basicity values at the firing temperature of 1,250°C. The basicity of briquettes in Figure 3(a)–(d) is 0, 0.67, 0.83, and 1.33, respectively. As shown in Figure 3(a), no slag phase was produced during firing, resulting in a relatively smooth mineral phase surface. With the increase of basicity, the porosity and the number of large pores in the briquettes gradually increased, as shown in Figure 3(b) and (c). When the basicity was greater than 0.83, the porosity in the briquettes did not increase, as shown in Figure 3(d).

Figure 3 SEM image of briquettes fired at 1,250°C with different basicity values (a) basicity = 0, (b) basicity = 0.33, (c) basicity = 0.83, and (d) basicity = 1.33.
Figure 3

SEM image of briquettes fired at 1,250°C with different basicity values (a) basicity = 0, (b) basicity = 0.33, (c) basicity = 0.83, and (d) basicity = 1.33.

Figure 4 shows the backscatter electron image of fired briquettes with different basicity values at 1,250°C. In Figure 4(a)–(d), the basicity values of briquettes are 0, 0.33, 0.83, and 1.33. When the basicity of briquettes is 0, a no-slag phase was observed but a few free SiO2 and a solution formed during firing, as shown in Figure 4(a). At the basicity of 0.33, a few slag and solution formed, as shown in Figure 4(b). The amount of solid solution in the briquette gradually increased when the basicity continued to rise, as shown in Figure 4(c) and (d).

Figure 4 Back scatter electron image of fired briquettes with different basicity values ① free SiO2; ② solution (a) basicity = 0, (b) basicity = 0.33, (c) basicity = 0.83, and (d) basicity = 1.33.
Figure 4

Back scatter electron image of fired briquettes with different basicity values ① free SiO2; ② solution (a) basicity = 0, (b) basicity = 0.33, (c) basicity = 0.83, and (d) basicity = 1.33.

Figure 5 shows the SEM images of fired briquettes at different temperatures with the basicity of 0.83. As shown in Figure 5(a) and (b), at low firing temperatures of 1,230 and 1,250°C, large amounts of solution and less slag had formed. Subsequently, the movement of Fe3+ was restricted and Fe2O3 recrystallization was not completed, thus reducing the volume of briquette shrinkage after firing and resulting in low briquette density and high porosity. When the firing temperature reached 1,280 and 1,300°C, as shown in Figure 5(c) and (d), considering the increase in firing temperature, the mass fraction of solid solution decreased, the amount of slag phase increased, and Fe3+ migration and Fe2O3 recrystallization were promoted. Subsequently, the continuous crystals between Fe2O3 became complete, the briquette volume further shrunk after firing, the internal structure of the briquettes became dense, and the porosity became low.

Figure 5 SEM images of fired briquettes at different firing temperatures (basicity = 0.83) (a) 1,230°C; (b) 1,250°C; (c) 1,280°C; (d) 1,300°C.
Figure 5

SEM images of fired briquettes at different firing temperatures (basicity = 0.83) (a) 1,230°C; (b) 1,250°C; (c) 1,280°C; (d) 1,300°C.

3.2 Influence of basicity on reducibility degree of fired briquettes

Figure 6 shows the effects of basicity on the reducibility of fired briquettes. The reducibility of briquettes fired at different temperatures increased and decreased with basicity, as shown in Figure 6. The reduction degree of firing briquettes was rapidly improved when the basicity was 0–0.83. As the basicity of briquettes continued to increase, the reduction degree of briquettes slightly changed. With the increase of firing temperature, the reduction degree of briquettes with different basicity decreased gradually. When the basicity of briquettes was 0.83 and the firing temperature was 1,230°C, the maximum reduction degree of the fired briquettes reached 56.68% in 60 min. When the basicity of briquettes was 0 and the firing temperature was 1,300°C, the minimum reduction degree of the fired briquettes reached 33.25% in 60 min.

Figure 6 Effects of basicity on the reducibility degree of the briquettes.
Figure 6

Effects of basicity on the reducibility degree of the briquettes.

Based on the comparison of the effects of firing temperature and basicity on the reducibility and porosity of fired briquettes, the reducibility of fired briquettes is positively correlated with the porosity of firing briquettes. When the basicity is in the range of 0–0.83, the porosity of the briquettes gradually increased and the contact area between the reducing gas and briquettes was enlarged, thus promoting the reduction reaction and the reduction degree. With the continuous increase of basicity (1.0–1.33), the porosity and the reduction degree of fired briquettes changed slightly. With the increase in firing temperature, the porosity of the briquettes decreased gradually and the tightness of the briquette microstructure was reduced. Subsequently, the contact area between the reducing gas and briquettes shrunk, the diffusion of reducing gas and reduction reaction was inhibited, and the reduction of briquettes was decreased.

3.3 Influence of basicity on RSI of fired briquettes

Figures 7–10 show the micromorphology of reduced briquettes at different basicity values fired at 1,230, 1,250, 1,280, and 1,300°C and then reduction for 60 min. With the increase of basicity, the size (diameter) of briquettes after reduction first increased and then decreased; and when the basicity was 0.83, the size of briquettes after reduction was the largest.

Figure 7 Morphology of reduced briquettes with different basicity values fired at 1,230°C and reduction for 60 min.
Figure 7

Morphology of reduced briquettes with different basicity values fired at 1,230°C and reduction for 60 min.

Figure 8 Morphology of reduced briquettes with different basicity values fired at 1,250°C and reduction for 60 min.
Figure 8

Morphology of reduced briquettes with different basicity values fired at 1,250°C and reduction for 60 min.

Figure 9 Morphology of reduced briquettes with different basicity values fired at 1,280°C and reduction for 60 min.
Figure 9

Morphology of reduced briquettes with different basicity values fired at 1,280°C and reduction for 60 min.

Figure 10 Morphology of reduced briquettes with different basicity values fired at 1,300°C and reduction for 60 min.
Figure 10

Morphology of reduced briquettes with different basicity values fired at 1,300°C and reduction for 60 min.

Figure 11 shows the effects of firing temperature and basicity on the swelling rate of fired briquettes. The swelling of briquettes after reduction increased and then decreased with basicity, and the swelling of briquettes after reduction was the largest when the basicity was 0.83. With the increase in firing temperature, the swelling rate of briquettes with different basicity values decreased gradually. When the basicity was 0.83, and the calcination temperature was 1,230°C, the swelling rate of the fired briquettes reached a maximum of 21.48% and catastrophic swelling was exhibited. However, when the basicity was 0 and the firing temperature was 1,300°C, the swelling rate of the fired briquettes was only 3.16%. When the basicity was less than 0.83, the porosity increased with the increase of basicity, which improved the kinetic conditions during reduction. At the same time, it also provided a site for the growth of iron whiskers and increased the reduction of swelling. When the basicity was greater than 0.83, the porosity does not change, but the amount of high melting point solid solution increased, which made the reduction difficult and the reduction swelling decreased.

Figure 11 Influence of basicity on the RSI of the briquettes.
Figure 11

Influence of basicity on the RSI of the briquettes.

3.4 Microstructures of the reduced briquettes after reduction

Figure 12(a)–(d) shows the SEM images of reduced briquettes with basicity of 0.83 at firing temperatures of 1,230, 1,250, 1,280, and 1,300°C and then reduction for 60 min. As shown in Figure 12(a), the metallic iron in the briquettes was mainly distributed in the form of whiskers with relatively close connections and a large number of iron whiskers. The swelling rate of the briquettes was 21.48%. When the firing temperature reached 1,250°C, the number of iron whiskers was relatively reduced, and the swelling rate of briquettes decreased to a certain extent, as shown in Figure 10(b). When the firing temperature reached 1,280°C, the number of whiskers was greatly reduced, and the morphology of whiskers changed from slender to stubby, in which the white particulate matter was mainly the solid solution formed by metal iron and silicon calcium, as shown in Figure 13. The swelling rate of briquettes decreased to 17.63%. When the firing temperature increased to 1,300°C, as shown in Figure 12(d), only a few of the metal Fe in the reduced briquettes showed short and coarse conical crystal structure; the compound was present in the form of layered metal Fe. The swelling rate of the briquettes was 12.68%.

Figure 12 SEM of reduced briquettes (R = 0.83) reduced for 60 min at different firing temperatures (a) 1,230°C, (b) 1,250°C, (c) 1,280°C, and (d) 1,300°C.
Figure 12

SEM of reduced briquettes (R = 0.83) reduced for 60 min at different firing temperatures (a) 1,230°C, (b) 1,250°C, (c) 1,280°C, and (d) 1,300°C.

Figure 13 EDS image of briquettes reduced for 60 min (basicity = 0.83).
Figure 13

EDS image of briquettes reduced for 60 min (basicity = 0.83).

Figure 14 shows the SEM images of briquettes with basicity values of 0, 0.33, 0.67, 0.83, 1.0, and 1.33 at a firing temperature of 1,250°C and then reduction for 60 min. After the reduction of briquettes with basicity of 0, the metal iron was distributed in the form of particles, which are relatively large and connected closely, as shown in Figure 14(a), and the swelling rate of briquettes was 7.24%. After the reduction of briquettes with basicity values of 0.33 and 0.67, the metal iron was no longer precipitated in the form of particles but was composed of a small number of particles, whiskers, and most of the network structure, in which the small white particles distributed on the network structure, were mainly the solid solution formed by metal iron and silicon calcium, as shown in Figure 14(b) and (c). Moreover, the swelling of briquettes increased to 8.06 and 12.86%. When the basicity values were 1.0 and 1.33, the iron whiskers after briquette reduction mainly had a stubby shape and iron whiskers mostly appeared in the pore sites with the growth of the pore, as shown in Figure 14(e) and (f), and the swelling rates of briquettes decreased to 18.03 and 15.83%.

Figure 14 SEM image of reduced briquettes with different basicity reduced for 60 min: (a) basicity = 0, (b) basicity = 0.33, (c) basicity = 0.67, (d) basicity = 0.83, (e) basicity = 1.0, and (f) basicity = 1.33.
Figure 14

SEM image of reduced briquettes with different basicity reduced for 60 min: (a) basicity = 0, (b) basicity = 0.33, (c) basicity = 0.67, (d) basicity = 0.83, (e) basicity = 1.0, and (f) basicity = 1.33.

4 Conclusion

As the basicity of briquettes increased, the volume and porosity of briquettes after firing increased gradually. When the basicity was greater than 0.83–1.00, the volume and porosity of briquettes slightly changed. After firing, the volume and porosity of fluxed briquettes decreased with increasing temperature. With the increase of briquette basicity, the amount of solution produced during briquette firing first decreased and then increased and the lowest value was reached when the basicity was 0.24. When the basicity was in the range of 0–0.83, the porosity in the briquettes increased rapidly with the increase in basicity, and this condition promoted the reduction reaction and the growth of iron whiskers. When the basicity of briquettes was greater than 0.83, the porosity of fired briquettes did not increase but the solution with a high melting point continued to increase, thus inhibiting the reduction reaction and the growth of iron whiskers. The reduction and swelling of briquettes were positively correlated with the porosity of briquettes. With the increase in firing temperature, the swelling of the briquettes decreased gradually and the precipitation morphology of the metallic iron in the briquettes gradually changed from whisker-shaped metallic iron to massive and layered metallic iron. The metal iron was generally distributed in large and tightly connected granules. The swelling was related to the shape of the reduced metal iron. When the morphology of the reduced iron was slender and a relatively dense whisker, the swelling of the briquettes was relatively high. The reduced metal iron was distributed in the form of particles or the whiskers were coarse and short, and the swelling of the briquettes was relatively low.

Acknowledgments

The authors wish to acknowledge gratefully the financial support provided by the National Science Foundation of China (Project No. 51774005) and Natural Science Research Project for Anhui Universities (No. KJ2018A0045).

  1. Funding information: Financial support provided by the National Science Foundation of China (Project No. 51774005) and Natural Science Research Project for Anhui Universities (No. KJ2018A0045).

  2. Author contributions: Wang Ping finished the results analysis. Wu Hao wrote the manuscript. Chun Tie-jun provided the technological idea and revised the manuscript. Zhou Song and Zhou Tian-bao carried out the experiment.

  3. Conflict of interest: Authors state no conflict of interest.

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Received: 2021-08-24
Accepted: 2021-12-06
Published Online: 2022-04-20

© 2022 Wang Ping et al., published by De Gruyter

This work is licensed under the Creative Commons Attribution 4.0 International License.

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https://doi.org/10.1515/htmp-2022-0023
Keywords for this article
fluxed briquettes; reduction swelling; porosity; iron whisker
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