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铬在Al2O3-SiO2-MgO-CaO-CrOx渣系与铬铁合金间的分配行为

铬在Al2O3-SiO2-MgO-CaO-CrOx渣系与铬铁合金间的分配行为

郭 宇峰，
李 志伟，
王 帅，
刘 飞，
陈 凤，
杨 凌志，
李 兆祥，
李 广，
杨 剑峰
中南大学学报（英文版）第32卷, 第2期pp.392-404纸质出版 2025-02-26
DOI：10.1007/s11771-025-5884-8
300

高碳铬铁是生产不锈钢的主要含铬原料，随着不锈钢需求量及产量的增加，对高碳铬铁的需求也日益提高。目前主要采用电炉冶炼法生产高碳铬铁，但该过程存在元素回收率低等问题。炉渣的物化性能对于高温冶炼过程元素回收及渣铁分离效果具有重要影响。因此，研究铬铁矿冶炼过程中Cr在炉渣和高碳铬铁合金之间的分配行为，优化渣系组成，提高元素回收率，对保障我国不锈钢产业的可持续发展意义重大。本论文以高碳铬铁合金电炉冶炼过程的Al2O3-SiO2-MgO-CrOx渣系为基础，研究了w(CaO)/w(SiO2)对Al2O3-SiO2-MgO-CaO-CrOx炉渣黏度的影响以及Cr在炉渣与高碳铬铁合金间分配行为的影响。采用FactSage 8.1计算了不同炉渣碱度条件下渣中Cr2O3与CrO的活度变化规律，以及不同温度下炉渣的相平衡关系和含铬物相中铬含量。在理论分析的基础上，开展了Cr在炉渣与高碳铬铁合金间分配行为的高温平衡验证实验，利用XRD、SEM-EDS等分析方法对渣铁样品进行了物相及微观结构分析。研究结果表明，Al2O3-SiO2-MgO-CaO-CrOx炉渣的主要物相为含铬尖晶石、镁铝尖晶石、镁橄榄石和钙镁橄榄石，随着炉渣中w(CaO)/w(SiO2)的提高，渣中尖晶石含量和尖晶石中CrOx含量下降，钙镁橄榄石的含量增加，镁橄榄石含量降低，炉渣的黏度降低，铬在Al2O3-SiO2-MgO-CaO-CrOx渣与铬铁合金间的分配比降低，且主要存在于尖晶石物相中。结果表明，提高炉渣的w(CaO)/w(SiO2)有利于促进Cr的还原迁移，降低炉渣中的Cr含量，有利于提高铬铁矿电炉冶炼过程Cr的回收率。

Al2O3-SiO2-MgO-CaO-CrOx渣尖晶石黏度铬分配比铬铁矿

1 Introduction

Chromium is an essential alloying element in stainless steel, which can improve the corrosion resistance of stainless steel [1, 2]. During the production of stainless steel, the high-carbon ferrochrome alloy is generally used to adjust the chromium content of the stainless steel [3, 4]. Generally, high-carbon ferrochrome alloy is mainly obtained by electric furnace smelting of chromite [5], and the slag is also obtained in the smelting process. The ferrochrome slag was mainly composed of molten oxides, chromium spinel, and metal droplets [6, 7]. The main components of molten oxides are SiO2, MgO, Al2O3, CaO and 6%-12%CrOx [8-10]. Due to the high content of MgO and Al2O3, and also the existence of CrOx, the slag viscosity is high [11-13], which makes it difficult to separate the slag from the alloy in production process, affecting the recovery rate of chromium [14, 15]. And the chromium-containing slag is not correctly disposed, which is harmful to the environment and ecology [16-18]. Therefore, increasing the distribution ratio of chromium between the alloy and slag to reduce the content of CrOx in slag is very important for environmental protection and improving chromium’s recovery rate.

At present, the slag in chromite smelt process mainly is MgO-Al2O3-SiO2-CrOx system [19, 20], and its main phases are magnesia-aluminum spinel and magnesia olivine [21]. Some studies reported that increasing the CaO content in the slag promoted the reduction of chromium in chromite [22, 23], and other studies have reported that increasing binary basicity could improve the recovery of chromium in laterite nickel ore [24, 25], so adding CaO can improve the recovery rate of Cr from ore, but the CaO content in slag will increase with adding of CaO. When binary basicity was 1.96, CrOx mainly existed as CaCr2O4 in the slag [26]; when binary basicity decreased to 0.96, CrOx would form a spinel phase with Mg, Al, Fe, and O, resulting in increasing content of Cr and Fe in the spinel phase and decreasing recovery rate of Cr [27-33]. Some studies have increased the content of SiO2 in the slag [15, 23, 24], which reduced the CrOx in the slag, but when the SiO2 content is too high, it prevents the combination of chromium and carbon, and the recovery rate of Cr is reduced [15, 23, 24, 34]. In addition, the influence of w(MgO)/w(Al2O3) on slag showed that when the content of MgO is less than 10%, the increase of w(MgO)/w(Al2O3) can decrease the viscosity of slag; when w(MgO) in slag is higher than 10%, the increase of w(MgO)/ w(Al2O3) can increase the viscosity of slag [35-37]. At the same time, some studies reported that the increase of w(MgO)/w(Al2O3) could increase the melting temperature of slag [38]. And the element recovery rate will be low when the viscosity and melting temperature of the slag are high [39-41]. In general, binary basicity w(CaO)/w(SiO2), w(MgO)/w(Al2O3), and w(SiO2) in slag would affect the recovery of Cr and the current research on the distribution of Cr between slag and alloy is listed in Table 1.

Table 1
Effects of chemical compositions on the distribution of elements in various CrOx containing slag systems
Slag systemResultRef.
CaO-MgO-Al2O3-SiO2w(CrOx) decreased in slag when w(SiO2)/w(Al2O3) increased from 2.25 to 5.50[15]
CaO-Al2O3-MgO-SiO2-CrOx-FexOw(CrOx) increased in slag when w(SiO2) increased from 5% to 15%[26]
CaO-SiO2-MgO-Al2O3-Cr2O3w(CrOx) increased in spinel when w(FeO) increased from 0% to 6%[32]
MgO-SiO2-FeO-Cr2O3-MnO-TiO2-V2O3w(CrOx) increased in slag when w(FeO) increased from 40% to 50%[42]
CaO-SiO2-MgO-Al2O3-CrOxw(CrOx) decreased in slag when temperature increased from 1450 to 1600 ℃, but increased when w(Al2O3) increased from 6% to 14%[43]
CaO-MgO-SiO2-Cr2O3w(CrOx) decreased in spinel when w(CaO)/w(SiO2) increased from 1.0 to 2.0, w(CaO)>50%[44]
CaO-MgO-SiO2-Cr2O3-Al2O3w(CrOx) decreased in spinel when w(Al2O3) increased from 3% to 12%[45]
CaO-MgO-Al2O3-SiO2

w(CrOx) increased in slag with w(SiO2) increased from 0% to 20%,

w(MgO)=5%

[46]
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As shown in Table 1, the effect of binary basicity w(CaO)/w(SiO2) on the Cr distribution ratio between CaO-MgO-Al2O3-SiO2-CrOx slag and alloy was not very clear.

Therefore, the purpose of this study is to investigate the effect of binary basicity w(CaO)/w(SiO2) on the distribution ratio of chromium between the high-carbon ferrochrome alloy and slag. The reaction thermodynamics, the activity of chrome-containing ion groups, and the slag viscosity are calculated by FactSage 8.1. In addition, the effects of slag basicity on the distribution behavior of chromium between the hot metal and slag are experimentally studied. These research results provide evidence for improving the recovery rate of chromium in the production of high-carbon ferrochrome by the electric furnace process.

2 Experimental

2.1 Materials

The raw materials used in this experiment included synthetic slag and high-carbon ferrochrome alloy. The synthetic slag was a mixture of chemically pure reagents MgO, Al2O3, SiO2, CaO, and Cr2O3. The slag composition is that the basicity (w(CaO)/w(SiO2)) was 0.2, 0.4 and 0.6, the w(MgO)/w(Al2O3) was 1.0, the w(SiO2) was 30% and the w(Cr2O3) was 5%. The used chemical reagents CaCO3 (pic99%), SiO2 (pic99.9%), Al2O3 (pic99%), MgO (pic99%), and Cr2O3 (pic99%) were calcined at 1000 ℃ in argon gas for 3 h to remove any moisture or carbonate that may exist in them.

In addition, the high-carbon ferrochrome alloy used was taken from a company. Table 2 lists the main composition of the alloy sample.

Table 2
Chemical composition of high carbon ferrochrome alloy
CCrPSSiFe
7.7351.870.0250.0252.7637.59
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2.2 Experimental methods

The analytical pure reagents MgO, Al2O3, SiO2, CaO and Cr2O3 were weighed according to the designed compositions and thoroughly mixed in an agate mortar for more than 30 min. The mixtures were placed into a carbon crucible lined with molybdenum flakes and then melted at 1500 ℃ for 0.5 h in a muffle furnace with the protection of high-purity argon gas (φ(Ar)>99.99%, P(O2)<10-1 Pa), and the gas flow rate was 1.0 L/min. Then, the pre-melted slag was taken out from the furnace and quenched in cold water to obtain synthetic slag. Subsequently, the synthetic slag (25 g) and the high-carbon ferrochrome alloy powder (25 g) were placed into the graphite crucible, the synthetic slag was placed on the bottom, and the alloy sample was placed on the slag. The graphite crucible was then put into a high-temperature muffle furnace. The muffle furnace (KJ GROUP Company: KSL-1700X-S) was used in experiment. The distribution experiments were carried out at 1650 ℃ for 30 min and then 1600 ℃ for 180 min with the protection of high-purity argon gas (φ(Ar)>99.99%) and the gas flow rate was 1.0 L/min to keep low partial pressure of oxygen. Then the samples were cooled with the furnace under argon atmosphere protection. Finally, the slag and alloy were separated and sampled for the following analysis.

2.3 Analysis methods

The phase composition of the slag samples was detected by XRD (Empyrean, PANalytical B.V, Cu-Kα radiation, 45 kV, 40 mA, Netherlands), with a diffraction angle (2θ) ranging from 3° to 100° as well as a step size of 0.002°. And the w(Cr) in the alloy, the w(Cr) and the w(Fe) in the slag were detected with chemical analysis (GB/T 4699.2—2008 and GB/T 24225—2009). The microstructure of slag was observed by SEM (TESCAN MIRA3-LMH), and phase components were measured by EDS (TESCAN Max 20, Oxford, UK).

The distribution ratio of Cr between alloy and slag is calculated by:

pic (1)

where w(Cr) represents the content of Cr in the alloy, and w(CrOx) represents the content of CrOx in the slag.

In addition, the FactSage 8.1 with module “Equilib” and “Viscosity” with the database “FactPS,” “FToxid”, and “FTmisc” was used to calculate the reaction thermodynamics of CaO-Al2O3-SiO2-MgO-CrOx slag system, the activity of chrome oxides and the viscosity of the slag systems.

Figure 1
(a) Experimental flow chart and (b) heat-treatment regimes in this experiment
pic

3 Results and discussion

3.1 Effect of basicity on a(CrOx) and Cr distributions

During the smelting process, the oxygen in the furnace is consumed by reducing substances, resulting in a low partial pressure of oxygen in the furnace, and its value is about P(O2)=10-5 Pa, and the slag contains Cr2+ and Cr3+ [47, 48]. Therefore, we calculated the activity of CrO and Cr2O3, and the activity of CrO and Cr2O3 in the slag with different basicity at different P(O2) was calculated using the “Equilib” module in FactSage 8.1 software. The activity results of Cr2O3 and CrO at different P(O2) are shown in Figures 2 and 3. The activity of CrO and Cr2O3 increases with the basicity at different oxygen partial pressures. This means that the effect of basicity on the activity of CrO and Cr2O3 is the same at different partial pressures of oxygen, which fully indicates that the increase of basicity promoted the reduction of Cr, improved the recovery of Cr from slag and reduced the content of CrOx in the slag.

Figure 2
Activity of CrO in slag with different basicity at different P(O2): (a) 10-1 Pa; (b) 10-3 Pa; (c) 10-5 Pa; (d) 10-7 Pa
pic
Figure 3
Activity of Cr2O3 in slag with different basicity at different P(O2): (a) 10-1 Pa; (b) 10-3 Pa; (c) 10-5 Pa; (d) 10-7 Pa
pic

The “Equilib” module in FactSage 8.1 was used to calculate the distribution ratio of Cr between the alloy and the slag. As shown in Figure 4, in the condition of the same w(MgO)/w(Al2O3), the distribution ratio of Cr between the alloy and slag increases with the increase of the slag basicity, which means that increasing slag basicity can increase Cr content in alloy and reduce Cr content in slag.

Figure 4
Effect of basicity on the distribution of Cr between alloy and slag
pic
3.2 Effect of basicity on phase transformation and w(CrOx) in different phases

Figure 5 shows the change of different phases in slag with temperature and slag basicity. It can be seen that the main phases are the liquid slag and spinel when the temperature is higher than 1600 ℃. The proportion of the liquid phase increases while the proportion of the spinel phase decreases with the increase of slag basicity, providing a good dynamic condition for Cr to enter the alloy from slag. Figure 6 illustrates the effects of temperature and basicity on the content of the spinel in slag. The content of the spinel in slag is high at low basicity and low temperature, but the increase of basicity or temperature is conducive to decreasing the content of spinel in slag.

Figure 5
The phase of slag with different basicity changes with different temperatures: (a) w(CaO)/w(SiO2)=0.2; (b) w(CaO)/w(SiO2)=0.4; (c) w(CaO)/w(SiO2)=0.6; (d) w(CaO)/w(SiO2)=0.8
pic
Figure 6
The variation of spinel with different basicity in slag
pic

Figures 7 and 8 show that the CrOx content in spinel and liquid slag decreases with the basicity increase, the CrOx content in liquid slag with low basicity is higher than liquid slag with high basicity at the same temperature. In addition, it can be seen that the phases in the slag are olivine, spina, and liquid slag when the temperature is higher than 1400 ℃ according to Figure 5, and the contents of olivine and spinel decrease, the content of liquid slag increases with temperature increases. The temperature of the production of high-carbon ferrochrome alloy is higher than 1600 ℃, Therefore, it is concluded that the content of spinel in slag, the CrOx content in liquid slag and spinel can be reduced simultaneously by increasing basicity. The reason why increasing basicity and temperature can improve the recovery rate of chromium may be that with the increase of basicity or temperature, the content of CrOx in spinel decreases, the spinel phase in slag gradually decreases, the CrOx diffuses into liquid slag from spinel, and liquid slag can fully contact with the alloy. The diffusion condition becomes better between liquid slag and iron, which provides a good condition for Cr to enter the alloy from the slag. And chromium can be infinitely dissolved in metal at high temperatures; the activity of CrOx in slag increases with the increase of basicity or temperature, promoting the diffusion of chromium from slag to alloy.

Figure 7
The variation of CrOx content with basicity in liquid slag and spinel
pic
Figure 8
Cr and CrOx content in different phases at 1650 ℃
pic
3.3 Distribution behavior of Cr with different basicity

Figure 9 shows the separation situation of alloy and slag under different basicity conditions. It can be seen that the separation of alloy from slag is successful, but there is a small part of slag samples on the surface of the alloy sample under low basicity conditions.

Figure 9
External view of alloy and slag at different basicity: (a) w(CaO)/w(SiO2)=0.2; (b) w(CaO)/w(SiO2)=0.4; (c) w(CaO)/w(SiO2)=0.6
pic

Table 3 shows the w(Cr) in alloy samples and w(CrOx) and total Fe in slag samples. When the basicity of slag is 0.2, 0.4, 0.6, the content of w(Cr) in the alloy is 47.97%, 49.48%, and 50.00%, respectively, while the content of w(CrOx) in the slag is 2.65%, 2.02%, and 0.29%, respectively. The content of w(CrOx) in slag decreases, and the distribution ratio of Cr between the alloy and slag increases gradually. Moreover, the total iron content in the slag increases with the increase of slag basicity. Figure 10 shows the XRD pattern of slags. The main phases are spinel, melilite and olivine according to the XRD pattern. The peaks of the melilite become stronger with the increasing slag basicity.

Table 3
Element content in slag and alloy
No.w(CaO)/w(SiO2)AlloySlagw(Cr)/w(CrOx)
w(Cr)w(CrOx)w(TFe)Calculated with experimental dataCalculated by FactSage 8.1
10.247.97%2.65%0.62%18.1043.51
20.449.48%2.02%0.39%24.5058.89
30.650.00%0.29%0.11%172.4180.39
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Figure 10
XRD spectra of slag samples
pic
3.4 Microstructure and phase composition of slag

Figure 11 shows the SEM diagram of slag with different basicity. It can be observed that low-basicity slag contains more white particles. According to the EDS analysis of slag, the white grains are high-carbon ferrochrome alloy particles. In addition, the amounts of alloy grains in higher basicity slag samples decrease, which can be judged that with the increase of basicity, the residual alloy samples in slag can be effectively reduced. As shown in Figure 12, it can be concluded that the reason may be that under the condition of low basicity, slag viscosity is high, the separation of slag and iron is difficult, resulting in incomplete separation of slag and iron, and there are more residual alloys in slag, resulting in reduced recovery of Cr.

Figure 11
SEM diagram of slag with different basicity: (a) w(CaO)/w(SiO2)=0.2; (b) w(CaO)/w(SiO2)=0.4; (c) w(CaO)/w(SiO2)=0.6
pic
Figure 12
Effect of w(CaO)/w(SiO2) on the slag viscosity (η) at different temperatures (a) and slag viscosity at 1650 ℃ (calculated by FactSage 8.1) (b)
pic

Figure 16 compares the influence of slag basicity on the distribution of chromium between slag and iron in different literature. As shown, the CaO-10%MgO-20%Al2O3-SiO2-CrOx system slag studied by WEI et al [15] and the CaO-FeO-Al2O3-SiO2-CrOx system slag studied by SIIMBI et al [49] are similar to the CaO-MgO-Al2O3-30%SiO2-CrOx system slag in this paper, it is verified that the improvement of basicity is conducive to the entry of chromium from the slag into the alloy, thus improving the recovery and utilization of chromium. However, the study of SHU et al [50], LI et al [26], ALBERTSSON et al [51] and others also showed that CrOx mainly existed in the state of chromium spinel in slag, and the increase of slag basicity reduced the content of CrOx in spinel.

Figure 13
SEM and EDS diagram of spinel in slag with basicity 0.2
pic
Figure 14
SEM and EDS diagram of spinel in slag with basicity 0.4
pic
Figure 15
SEM and EDS diagram of spinel in slag with basicity 0.6
pic
Figure 16
Comparison the data of different works and this paper: (a) w(CrOx) in slag; (b) w(CrOx) in spinel
pic

4 Conclusions

The effect of basicity of CaO-MgO-Al2O3-SiO2-CrOx slag on the distribution ratio of chromium between alloy and slag was studied. The increase of basicity in the CaO-MgO-Al2O3-SiO2-CrOx slag promoted chromium to enter the alloy from the slag. The thermodynamic calculation showed that the increase of basicity in CaO-MgO-Al2O3-SiO2-CrOx slag increased the activity of CrOx in the smelting process so that CrOx was more easily separated from the spinel phase. The increase of basicity reduced the slag viscosity, which is conducive to diffusion and transmission between alloy and slag, and promoted the recovery of chromium. In addition, the SEM and EDS results showed that the main phases in the slag were chrome-spinel, magnesia-alumina spinel, magnesia olivine, and calcium-magnesia olivine. With the increase of basicity, the calcium-magnesia-olivine phase and magnesia-alumina spinel phase in the slag increased while the spinel phase decreased. The alloy phase in the slag was reduced, and the slag iron separation was more complete, leading to a higher recovery rate of Cr.

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注释

The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.

GUO Yu-feng, LI Zhi-wei, WANG Shuai, LIU Fei, CHEN Feng, YANG Ling-zhi, LI Zhao-xiang, LI Guang, YANG Jian-feng. Distribution behavior of Cr between high-carbon ferrochrome alloy and Al2O3-SiO2-MgO-CaO-CrOx slag [J]. Journal of Central South University, 2025, 32(2): 392-404. DOI: https://doi.org/10.1007/s11771-025-5884-8.

郭宇峰,李志伟,王帅等.铬在Al2O3-SiO2-MgO-CaO-CrOx渣系与铬铁合金间的分配行为[J].中南大学学报（英文版）,2025,32(2):392-404.

论文推荐

1 Introduction

2 Experimental

2.1 Materials

2.2 Experimental methods

2.3 Analysis methods

3 Results and discussion

3.1 Effect of basicity on a(CrOx) and Cr distributions

3.2 Effect of basicity on phase transformation and w(CrOx) in different phases

3.3 Distribution behavior of Cr with different basicity

3.4 Microstructure and phase composition of slag

4 Conclusions

References

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