<bold>Fe2O3-CaO-TiO2 </bold>体系下铁酸钙的合成过程及<bold>TiO2 </bold>和<bold>CaTiO3 </bold>的影响

程功金; 周新磊; 高明磊; 常富增; 滕艾均; 邢振兴; 宋翰林; 高子先; 汤卫东; 赵备备; 王金龙; 赵丹; 刘超; 李兰杰; 杨合; 陈东辉; 薛向欣; 白瑞国; 张卫军; Cheng Gongjin; Zhou Xinlei; Gao Minglei; Chang Fuzeng; Teng Aijun; Xing Zhenxing; Song Hanlin; Gao Zixian; Tang Weidong; Zhao Beibei; Wang Jinlong; Zhao Dan; Liu Chao; Li Lanjie; Yang He; Chen Donghui; Xue Xiangxin; Bai Ruiguo; Zhang Weijun

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Synthesized Process of Calcium Ferrite and Effect of TiO₂ and CaTiO₃ in Fe₂O₃-CaO-TiO₂ System PDF

- ORCID：
Cheng Gongjin ^1,2
- ORCID：
Zhou Xinlei ³
- ORCID：
Gao Minglei ⁴
- ORCID：
Chang Fuzeng ⁴
- ORCID：
Teng Aijun ⁵
- ORCID：
Xing Zhenxing ¹
- ORCID：
Song Hanlin ¹
- ORCID：
Gao Zixian ¹
- ORCID：
Tang Weidong ¹
- ORCID：
Zhao Beibei ⁴
- ORCID：
Wang Jinlong ⁴
- ORCID：
Zhao Dan ⁴
- ORCID：
Liu Chao ⁴
- ORCID：
Li Lanjie ⁴
- ORCID：
Yang He ^1,2
- ORCID：
Chen Donghui ⁴
- ORCID：
Xue Xiangxin ^1,2
- ORCID：
Bai Ruiguo ⁴
- ORCID：
Zhang Weijun ¹

1. School of Metallurgy, Northeastern University, Shenyang 110819, China； 2. Liaoning Key Laboratory of Recycling Science for Metallurgical Resources, Shenyang 110819, China； 3. Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110819, China； 4. HBIS Group ChengSteel, Chengde 067102, China； 5. Ansteel Beijing Research Institute, Beijing 102200, China

Updated：2021-07-08

Abstract

In order to investigate the phenomenon that the affecting mechanism of high-titanium vanadium-titanium magnetite is caused by separate TiO₂ or by CaTiO₃ formed from TiO₂ and CaO, calcium ferrite was synthetized by pure reagents of Fe₂O₃ and CaO, and the effect of TiO₂ and CaTiO₃ on the formation mechanism of titanium calcium ferrite (FCT) was researched. Different samples were sintered at the temperatures of 1023~1423 K for different time under air atmosphere based on thermodynamics calculations with Factsage 7.0. The phase transformation and microstructure changes in sintered samples were examined through different characterization means including X-ray diffraction and scanning electron microscope-energy disperse spectroscopy. It is found that the formation process of calcium ferrite can be mainly divided into two stages. The synthesized product is Ca₂Fe₂O₅ with the reaction “Fe₂O₃ (s) + 2CaO (s) = Ca₂Fe₂O₅ (s)” between Fe₂O₃ and CaO at 1023~1223 K in the former stage, and the predominant product is CaFe₂O₄ with the reaction “Ca₂Fe₂O₅ (s) + Fe₂O₃ (s) = 2CaFe₂O₄ (s)” between Ca₂Fe₂O₅ and Fe₂O₃ at 1223~1423 K in the latter stage, in which the reaction rate is accelerated especially at 1423 K. It is observed that CaTiO₃ increases with increasing the temperature. However, the solid solution of Ti element in calcium ferrite is greatly difficult to realize and the reaction between TiO₂ and calcium ferrite is not an effective way to generate FCT. It is also observed that the amount of Fe element in the phase boundary of CaTiO₃ and FCT increases with the extension of the thermal insulation time. FCT is predominantly formed through the solid solution of Fe component in CaTiO₃, and the main reaction is “Fe₂O₃ (s) + CaTiO₃ (s) = FCT (s)”.

Keywords

calcium ferrite; sintering; TiO₂; CaTiO₃; Fe₂O₃-CaO-TiO₂ system

Vanadium-titanium magnetite, rich in iron, titanium, vanadium, etc, has significant comprehensive utilization value and is used widely in the blast furnace iron-making and latter vanadium-extracting industry in China so far^[

1-6]. It has been reported comprehensively that the tumbler strength, rate of finished products and low temperature reduction and pulverization rate of vanadium-titanium magnetite sinters are greatly poor, and previous studies have indicated that TiO₂ has great reverse effects on the sinter quality of vanadium-titanium magnetite^{[Reference 7

Baidu Scholar}7,8]. However, researchers have different opinions on the affecting mechanism of vanadium-titanium magnetite sinters^{[Reference 8

Baidu Scholar}8,9] and it is still unclear that the deterioration of sinter property is caused by separate TiO₂ or CaTiO₃ formed from TiO₂ and CaO.

For ordinary iron ores, it is commonly affirmed that the strength increasing of iron ore sinters has great relations with the generation of calcium ferrite, and calcium ferrite theory provides theoretical basis for the production of modern high basicity sinters with good quality^[

10-12].However, for vanadium-titanium magnetite ores, calcium ferrite is evidently found less but perovskite (CaTiO₃), Fe-bearing anosovite (Fe_0.5Mg_0.5Ti₂O₅) are obviously found because of the existence of TiO₂ in the sinters, contributing to the complexity of sintering consolidation and liquid reaction mechanism. Since calcium ferrite theory cannot explicitly illustrate the low strength, poor quality and especially serious reduction degradation, the challenge is proposed for the applicability of traditional calcium ferrite theory. Consequently, it is necessary to research the effect of TiO₂ and CaTiO₃ on the formation mechanism of titanium-bearing calcium ferrite.

High-titanium vanadium-titanium magnetite ores have relatively far higher titanium contents compared with ordinary vanadium-titanium magnetite^[

13]. As the largest high-titanium vanadium-titanium magnetite, 20 billion tons of reserves have just been explored in Chaoyang District in Liaoning of China in recent several years, which accounts for more than half of total vanadium-titanium magnetite resources in China. Large-scale exploitation and utilization of these mineral resources have seldom been carried out so far due to the poor-quality sinters and immature utilization technology. Compared with or-dinary vanadium-titanium magnetite, the influencing of titanium oxide on vanadium-titanium magnetite is more highlighted.

According to the theory of calcium ferrite, researchers have done lots of work focusing on the optimization of sinters for ordinary iron ores. Ding et al have studied the formation mechanism of silicon-ferrite of calcium (SFC) by solid-state reactions in order to understand the process of SiO₂ involved in the formation of complex silico-ferrites of calcium and aluminum^[

14], and Pownceby et al have investigated the solid solution limits, thermal stability and selected phase relationships within the Fe₂O₃-CaO-SiO₂ (FCS) system^{[Reference 15

Baidu Scholar}15]. Wang et al have researched the formation characteristics of calcium ferrite in low silicon sinter^{[Reference 16

Baidu Scholar}16]. Nakashima et al have researched the effects of adding SiO₂ or Al₂O₃ on the wetting and penetration characteristics of calcium ferrite melts, CaO·Fe₂O₃ (CF) and CaO·2Fe₂O₃ (CF₂) in sintered hema-tite^{[Reference 17

Baidu Scholar}17]. Besides, Jeon has studied the formation of calcium ferrites by solid state reactions between different kinds of iron oxides (Fe₂O₃, Fe₃O₄ and wustite) and CaO under various oxygen potentials at 1273 K^{[Reference 18

Baidu Scholar}18]. Yu et al have investigated the wetting behavior of MgO-doped and Al₂O₃-doped calcium ferrites^{[Reference 19

Baidu Scholar}19,20]. In addition, studies on the thermodynamic investi-gation^{[Reference 21

Baidu Scholar}21] and isothermal and non-isothermal reduction kinetics of MgO-doped, Al₂O₃-doped and SiO₂-doped calcium ferrites have been carried out^{[Reference 11

Baidu Scholar}11,22-24]. However, systematic studies on the formation mechanism of vanadium-titanium magnetite including high-chromium vanadium-titanium magnetite and high-titanium vanadium-titanium magnetite has been elusive. Chen et al has carried out the work on the diffusion behavior between Cr₂O₃ and calcium ferrite in order to provide theore-tical basis for the utilization of high-chromium vanadium-titanium magnetite^{[Reference 25

Baidu Scholar}25], and Ding et al have investigated the reaction sequence and formation kinetics of perovskite by calcium ferrite-titania reaction^{[Reference 26

Baidu Scholar}26]. However, effect of TiO₂ or formed CaTiO₃ on the formation of calcium ferrite in Fe₂O₃-CaO-TiO₂ (FCT) system is still unclear. Thus, it is essential and significant to figure out the effects of TiO₂ and CaTiO₃ on the formation mechanism of FCT phase.

In this study, the synthesized process of calcium ferrite was first studied by pure reagents of Fe₂O₃ and CaO, and the effect of TiO₂ and CaTiO₃ on the formation mechanism of FCT was further investigated. It is expected to provide theoretical guidance for vanadium-titanium magnetite sinter, especially high-titanium vanadium-titanium magnetite sinter.

1 Experiment

1.1 Experimental materials and methods

The pure reagents of Fe₂O₃, TiO₂ and CaO, provided by Sinopharm Chemical Reagent Co., Ltd, were adopted as the raw materials. The raw materials were weighed according to the ingredient scheme in Table 1, and mixed for 12 h with the agate ball. For each experimental sample, 3 g mixed materials were taken and pressed into a cylinder with the diameter of 8 mm and the height of 5 mm by briquetting machine under the pressure of 2.0 MPa for 2 min. The prepared samples were placed in the alumina crucible with 15 mm in diameter and 20 mm in height and then put in the Box-type atmosphere furnace for sintering with the temperature regime shown in Fig.1. Different samples were sintered and prepared in the selected temperatures of 1023, 1123, 1223, 1323 and 1423 K under air atmosphere.

Table 1 Ingredient scheme of solid-reaction (wt%)

Sample	Composition of raw materials			Content of elements
Sample	Fe₂O₃	CaO	TiO₂	Fe	Ca	Ti
1#	51	49	0	35.7	35	0
2#	49	43	8	34.3	30.7	6

Fig.1 Heating curve of sintering for different samples

1.2 Characterization methods

In this study, the sintered samples were ground to 0.05 mm in the grinding machine for X-ray diffraction (X-ray diffraction) analysis by X'pert pro (Panalytical, Almelo, the Netherlands) with Cu Kα radiation, and sanded and polished to a smooth surface for SEM examination and EDS analysis (scanning electron microscopy-energy dispersive spectros-copy, Ultra Plus; Carl Zeiss GmbH, Jena, Germany). XRD, SEM and EDS were used for the mineral phase analysis, the microscopic morphology examination and micro-area com-ponent investigation, respectively.

2 Results and Discussion

2.1 Formation process of calcium ferrite

Solid reaction is the most vital approach for the formation of FC, and the conditions of the solid reaction determine the phase types. Fig.2 describes XRD patterns of sample 1# (51wt%Fe₂O₃-49wt%CaO) sintered at 1023, 1123, 1223, 1323 and 1423 K for 2 h under air atmosphere. The results show that Ca₂Fe₂O₅(C₂F) appears at 1023 K, and the formation of C₂F is due to the reaction of Fe₂O₃ and CaO, as shown in Eq.(1).

Fig.2 XRD patterns of sample 1# (51wt%Fe₂O₃-49wt%CaO) sin-tered from 1023 K to 1423 K for 2 h under air atmosphere

Fe₂O₃ (s)+2CaO (s)=Ca₂Fe₂O₅ (s),

ΔG^θ=-53100-2.51T (J/mol)

(1)

The value of diffraction peak of Ca₂Fe₂O₅ increases obvi-ously with increasing the temperature, and some relatively weak diffraction peaks of Ca₂Fe₂O₅(C₂F) appear once again when the temperature increases to 1223 K, from which it is also indicated that the content of Ca₂Fe₂O₅increases as the temperature increases. Furthermore, the phase of CaFe₂O₄ appears at 1123 K and the content of CaFe₂O₄ begins to increase at 1223 K observably from XRD results. Ding et al^[

27] studied SiO₂ involved in the formation process of SFC by adopting XRD, in which it is reported that Ca₂Fe₂O₅ begins to form at 973 K while CaFe₂O₄ appears at 1073 K appro-ximately. In this study, talking the phase existence of Ca₂Fe₂O₅ at 1023 K (>973 K) and CaFe₂O₄ at 1123 K (>1073 K) does not represent to deny the lowest forming temperature, and it is mainly aimed at illustrating the formation process of C₂F in the temperature range of 1023~1223 K and that of CF at 1223~1423 K, in which both temperature ranges are higher than the lowest forming temperature of C₂F (973 K) and CF (1073 K) reported in Ding's study. In future study, the lower-ing temperature and temperature range will be researched.

Fig.3 shows SEM images of microscopic structures of sample 1# (51wt%Fe₂O₃-49wt%CaO) sintered at 1023 and 1423 K for 2 h under air atmosphere. The voids and holes in Fig.3c are formed probably because solid particles that do not participate in the reaction are dropped from the reacted sample during SEM-EDS sample preparation. Through the micros-copic structures analysis of samples, it can be found that the bonding phase is mainly Ca₂Fe₂O₅(FC₂) at 1023 K, and there are still intermediate mixing phases (circled part in Fig.3b and 3d) containing Fe³⁺, Ca²⁺ and O^2- for forming calcium ferrite phases. Due to solid-state reaction, Ca₂Fe₂O₅ will continue to react with Fe₂O₃ which is not involved in the reaction in the case that Fe₂O₃ is abundant. The reaction process between FC₂ and Fe₂O₃ is given by Eq.(2).

Fig.3 SEM images of microscopic structures for sample 1# (51wt%Fe₂O₃-49wt%CaO) sintered at 1023 K (a, b) and 1423 K (c, d) for 2 h under air atmosphere

Ca₂Fe₂O₅ (s)+Fe₂O₃ (s)=2CaFe₂O₄ (s),

ΔG^θ=-6300-7.11T (J/mol)

(2)

Fig.4a and 4b show EDS results of sample 1# sintered at 1023 and 1423 K, respectively, in which areas A and B are FC₂ and FC phases, respectively. It is easy to find that the content of Fe element in the generated FC₂ is low at 1023 K. When the temperature increases to 1423 K, the content of Fe element in the generated FC₂ increases significantly, which indicates that Fe₂O₃ continues to participate in the formation process of FC with increasing the temperature.

Fig.4 EDS analysis results of FC phases for sample 1# sintered at 1023 K (a) and 1423 K (b)

Through above analyses, it can be concluded that the formation of calcium ferrites is dynamic, and this process is mainly divided into three steps. The first step is the reaction between Fe₂O₃ and CaO at 1023 K, and the reaction product is Ca₂Fe₂O₅, as shown in Eq.(1). When the temperature increases to 1223 K, the reaction in the second step between Ca₂Fe₂O₅ and Fe₂O₃ begins to occur, and the main product is CaFe₂O₄, as shown in Eq.(2). The reaction in the third step happens also between Fe₂O₃ and CaO at 1223 K, but what's different from the first step is that the resultant is CaFe₂O₄, as shown in Eq.(3).

CaO (s)+Fe₂O₃ (s)=CaFe₂O₄ (s),

ΔG^θ=-29700-4.81T (J/mol)

(3)

And the third reaction rate is accelerated when the temperature increases to 1423 K. Temperature is a very important factor in the generating process of FC. With the increase of temperature, the thermodynamic conditions are improved actively, and the solid reaction rate is accelerated. It is a pivotal cause of temperature influencing the reaction process.

2.2 TiO₂ role in generating process of FCT

Fig.5 shows XRD patterns of samples 2# (8wt%TiO₂-49wt%Fe₂O₃-43wt%CaO) that were sintered from 1023 K to 1423 K for 2 h under air atmosphere. The results show that there are small amounts of CaTiO₃ (CT) and Ca₃Fe₂TiO₈ (FCT) at 1023 K besides Ca₂Fe₂O₅(C₂F) and CaFe₂O₄(FC). Moreover, the peak intensity of CaTiO₃ and Ca₃Fe₂TiO₈ (FCT) (at 2θ of about 47° and 60°) increases as the temperature increases, indicating that the contents of CaTiO₃ (CT) and Ca₃Fe₂TiO₈ (FCT) increase with increasing the temperature.

Fig.5 XRD patterns of samples 2# sintered at 1023~1423 K for 2 h under air atmosphere

Besides, Ca₂Fe₂O₅ (C₂F) phase content increases to some extent, which is consistent with the previous description. The increase of CaTiO₃ is in accordance with previous study on the relationship between the contents of CaTiO₃ and tempe-rature^[

28]. For TiO₂, the most important way to participate is in the reaction process between TiO₂ and CaO, and CaTiO₃ is directly produced (Eq.(4)). For Ca₂FeO₅ (C₂F), the reaction between TiO₂ and Ca₂Fe₂O₅ (C₂F) (Eq.(5)) cannot be ignored.

CaO (s)+TiO₂(s)=CaTiO₃ (s),

ΔG^θ=-79900-3.35T (J/mol)

(4)

Ca₂Fe₂O₅ (s)+TiO₂(s)=CaTiO₃(s)+CaFe₂O₄ (s),

ΔG^θ=-56500-5.65T (J/mol)

(5)

From thermodynamics calculation, Eq.(5) is much easier to occur than other reactions (Fig.11). In other words, because of reaction of Eq.(5), although Ca₂Fe₂O₅ (C₂F) is generated in Eq.(1), some Ca₂Fe₂O₅ products are consumed again some-times, contributing to the slow increasing content of Ca₂Fe₂O₅ (C₂F). Another unsolved problem is the generating progress of Ca₃Fe₂TiO₈ (FCT), which will be further discussed.

Fig.6 SEM images of samples 2# sintered at different temperatures for 2 h under air atmosphere: (a) 1023 K, (b) 1123 K, (c) 1223 K, (d) 1323 K, and (e) 1423 K

Fig.7 SEM image (a) and EDS analysis of area A (b) and area B (c) in Fig.7a for the sample sintered at 1223 K for 2 h under air atmosphere

Fig.8 XRD patterns of FC sintered at 1473 K for 4 h under air atmosphere

Fig.9 XRD pattern of the reaction product between FC and TiO₂ carried out at 1423 K for 2 h

Fig.10 EDS analyses of area A (a), area B (b) and area C (c) for the reaction between FC and TiO₂

Fig.11 Thermodynamics data for different reactions

Fig.6 shows SEM images of microscopic structures of samples 2# that were sintered from 1023 K to 1423 K for 2 h under air atmosphere. It is observed that the content of the bonding phase increases gradually as the temperature increases. Besides, layers are present around FC when the temperature increases to 1223 K (Fig.6a~6c), so it can be determined that the composition of the layer is FCT through EDS analysis shown in Fig.7. The appearance of FCT layer has an important guiding role in understanding the effect of TiO₂ on the formation of FCT. There are two main approaches to form FCT layers that are present around FC. The first approach is the reaction between FC and TiO₂, and the second approach is the reaction between Fe₂O₃ and CT. However, the significant question that how FC is involved in FCT generating is unclear. Thus, these two important processes will be further elaborated in the following studies.

2.3 Calcium ferrite role in generating process of FCT

In order to further determine how calcium ferrite is invol-ved in the generating of FCT, reaction experiments between calcium ferrite and TiO₂ were carried out at 1423 K for 2 h, in which calcium ferrite was obtained by solid reaction at 1473 K for 4 h under air atmosphere, according to XRD pattern in Fig.8, and XRD results of the experiment are shown in Fig.9. From the results, the products include CaTiO₃ (CT), Ca₂Fe₂O₅ (C₂F) and Ca₃Fe₂TiO₈(FCT). In the process of preparing FC, parts of Fe₂O₃ and CaO are not fully involved in the reaction. As the particle sizes of Fe₂O₃ and CaO are not inhomo-geneous, contactile parts preferentially react while non-exposed parts have no chemical changes in a certain reaction time. Therefore, partial CaTiO₃ (CT) phases in the experiment

are caused by the reaction between TiO₂ and CaO, and partial FCT phases in the experiment are caused by the reaction between Fe₂O₃, TiO₂ and CaO. The source of Ca₂Fe₂O₅ (C₂F) phase comes from the reaction between Fe₂O₃ and CaO.

Fig.10 shows the EDS analysis results for the reaction between calcium ferrite and TiO₂ that was carried out at 1423 K for 30, 60 and 120 min. From the results, it is easy to find that the content of Ti element is very low and it gradually increases as the reaction time is prolonged, which means that the solid solubility of Ti element in calcium ferrite is limited. In other words, it is very difficult to generate FCT by the reaction between calcium ferrite and TiO₂ because the solid solution process of Ti element in calcium ferrite is greatly difficult to realize.

Fig.11 shows relationships between Gibbs free energy change and reaction temperature (the thermodynamics data was taken from Factsage 7.0). In terms of thermodynamics, the Gibbs free energy for Eq.(6), namely, for the reaction between CaFe₂O₄ and TiO₂, is much lower than that of other reactions at the same temperature, indicating that reaction of Eq.(6) is easier to realize in the temperature increase process. Therefore, although FCT is not formed by the reaction between TiO₂ and FC, Eq. (6) at 1423 K is facilitated.

TiO₂ (s)+CaFe₂O₄ (s)=CaTiO₃ (s)+Fe₂O₃ (s),

ΔG^θ = -50200 + 1.46T (J/mol)

(6)

2.4 CaTiO₃ role in generating process of FCT

In order to understand clearly the role of CaTiO₃ in the generating process of FCT, the reaction between CT and Fe₂O₃ was carried out at 1423 K for different time. Fig.12 shows XRD results of the reaction between CT and Fe₂O₃ at 1423 K for 30, 60 and 120 min. The results show that the products are mainly FCT, and it is indicated that another main route of the formation of FCT is through the reaction between CT and Fe₂O₃.

Fig.12 XRD patterns for reaction between CT and Fe₂O₃ at 1423 K for 30, 60 and 120 min

The SEM images of microscopic structures of different samples that were sintered at 1423 K for 30, 60 and 120 min are shown in Fig.13 and EDS results of FCT phases (areas A, B and C) are shown in Fig.14. It can be found that the amount of Fe element in FCT gradually increases with extension of thermal insulation time. Similarly, EDS line scanning analysis in Fig.15 shows the phase boundary between CT and FCT at 1423 K, which also shows similar experimental result. It is observed that the amount of Fe element in the phase boundary of CT and FCT increases with the extension of the thermal insulation time.

Fig.15 EDS line scanning results of the phase boundary between CT and FCT at 1423 K for 30 min (a) and 120 min (b)

The above analysis shows that the crucial way to generate FCT is the solid solution of Fe in CaTiO₃ (CT). It is probably as a result of the fact that Fe occupies the position of Ti in crystal lattice in the formation of FCT. The reaction process between CaTiO₃ and Fe₂O₃ is given by Eq.(7).

Fe₂O₃ (s) + CaTiO₃ (s) = FCT (s)

(7)

3 Conclusions

1) The formation process of calcium ferrite (FC) can be divided into two stages. The reaction product is Ca₂Fe₂O₅ between Fe₂O₃ and CaO at 1023~1223 K in the former stage. The predominant product is CaFe₂O₄ for the reaction between Ca₂Fe₂O₅ and Fe₂O₃ at 1223~1423 K in the latter stage, in which the reaction rate is accelerated especially at 1423 K.

2) The reaction between TiO₂ and FC is not an effective way to generate titanium calcium ferrite (FCT) at 1423 K because the solid solution of Ti element in FC is greatly difficult to realize. TiO₂ is mainly involved in reaction TiO₂ (s) + CaFe₂O₄ (s) = CaTiO₃ (s) + Fe₂O₃ (s) at 1423 K.

3) The main reason for the formation of FCT is the solid solution of Fe element in CaTiO₃, and the main reaction is that FCT is generated by Fe₂O₃ and CaTiO₃.

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Synthesized Process of Calcium Ferrite and Effect of TiO₂ and CaTiO₃ in Fe₂O₃-CaO-TiO₂ System PDF

Abstract

Keywords