Ceramics International 48 (2022) 11192–11198

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Ceramics International
journal homepage: www.elsevier.com/locate/ceramint

Evaluation of remelting low-fluxing ferrotitanium slag as a potential

refractory raw material: Thermal characteristics and stability
Yichong Li a, Huizhong Zhao a, *, Jiuhong Ma a, Yu Wang a, Han Zhang a, Jun Yu a, Li Feng b,
Yanli liu b
a
The State Key Laboratory of Refractories and Metallurgy, Wuhan University of Science & Technology, Wuhan, 430081, China
b
Jinzhou Guotai Industrial Co., Ltd., Jinzhou, 121000, China

A R T I C L E I N F O A B S T R A C T

Keywords: To effectively promote the utilization of metallurgical waste slag, studies on the characteristics and stability of
Titanium–alumina slag waste slag are essential for waste reuse. Ferrotitanium slag is a byproduct of smelting ferrotitanium with thermite
Ferrotitanium slag reduction. Low-fluxing ferrotitanium slag (LFS) is the main type of dumping slags produced by ferrotitanium
Refractory raw material
smelting. In this study, an electric arc furnace was used to prepare remelting LFS (RLFS) for homogenization and
Thermal stability
impurity removal. The characteristics and thermal stability of RLFS as a refractory raw material were charac­
terized. The thermal stability of RLFS was tested under different working conditions. A phase-structure transition
mechanism of RLFS particles was established according to the thermal stability test and thermodynamic cal­
culations. The Al2O3 content in RLFS exceeded 80%, and RLFS had lower thermal conductivity than brown
corundum, but a similar thermal expansion coefficient. The results show that RLFS is a suitable substitute for
corundum raw material; the thermal stability test results show that RLFS was susceptible to crack propagation in
an oxidizing environment above 1280 ◦ C. The findings of this research provide suggestions for the utilization of
RLFS to improve the application stability of refractory products using recycled raw materials.

1. Introduction of added quicklime, ferrotitanium slag can be divided into two types:
low-fluxing ferrotitanium slag (LFS; CaO content ≤9 wt%) and
Thermite reduction, which uses metal aluminum powder to reduce total-fluxing ferrotitanium slag (TFS; CaO content ≥9 wt%). The main
the ilmenite concentrate, has been used in ferrotitanium production for chemical components of LFS and TFS are the Al–Ti–O and Ca–Al–Ti–O
decades. Ferrotitanium slag, the byproduct of smelting, is separated systems, respectively. The main phases in LFS are corundum (Al2O3) and
from the alloy by taking advantage of their different specific gravities, titanium suboxides (TiO, Ti2O3), and the main phase of TFS is Ca(Al,
and the ratio of slag to alloy is approximately 1.5:1 [1–3]. The problems Ti)12O19 [9].
of environmental pollution and land use originating from open dumping With the increased public awareness of solid waste management in
of ferrotitanium slag require an urgent solution. Owing to technological recent years, increasing amounts of industrial slags have been recycled
developments in ferrotitanium smelting, the slags produced by different and reused as sustainable materials [10–14]. A considerable volume of
processes show different physical and chemical characteristics; there­ refractory products is consumed every year owing to mechanical wear
fore, customized solutions for the recycling and management of slags and slag erosion, which has led to a great demand for refractory raw
produced by different processes are required. In the current production materials [15,16]. The prices of traditional refractory raw materials
process, quicklime(CaO) is added as a fluxing agent to increase slag continue to rise owing to the gradual depletion of mineral resources and
fluidity, which makes it easier to separate the alloy from the slag [4,5]. increasingly stringent environmental policies [17]. This has made sus­
Because of its strong alkalinity, quicklime inhibits the compound reac­ tainable materials, which are recovered from solid waste, a promising
tion of TiO (an intermediate product of smelting) and Al2O3, which re­ option for refractory raw materials in recent years [18–21]. Owing to its
sults in a lower concentration of titanium suboxides in the slag, and high refractoriness (above 1580 ◦ C), low thermal conductivity, high
subsequently increases the alloy yield [6–8]. Depending on the amount alumina content (above 75 wt%) in chemical composition, and rich

* Corresponding author.
E-mail address: wustnano@163.com (H. Zhao).

https://doi.org/10.1016/j.ceramint.2021.12.339
Received 17 November 2021; Received in revised form 28 December 2021; Accepted 29 December 2021
Available online 1 January 2022
0272-8842/© 2022 Elsevier Ltd and Techna Group S.r.l. All rights reserved.
Y. Li et al. Ceramics International 48 (2022) 11192–11198

Table 1
Chemical composition of LFS (wt%).
Table 2
SiO2 Al2O3 Fe2O3 CaO TiO2 LOI Chemical composition of RLFS (wt%).
LFS 0.91 74.95 1.62 0.65 20.51 − 2.90 SiO2 Al2O3 Fe2O3 CaO TiO2 LOI

RLFS 0.27 80.27 0.16 0.72 17.13 − 1.16

calcium hexaaluminate phase, TFS is reused as a type of high-alumina
refractory raw material called calcium alumino-titanate [22–24].
Every year in Jinzhou, China, nearly 50,000 t of TFS produced from the Table 3
smelting of ferrotitanium alloys is recycled and sold into the refractory Physical properties of RLFS, TFS, and brown fused alumina.
raw material market as a substitute for bauxite. Previous research found Bulk Apparent Microhardness Refractoriness
that LFS is a type of ferrotitanium slag with corundum (Al2O3) and density porosity
low-valent titanium oxides (Ti2О3, TiO) as the main components, with a RLFS 3.92 g/ 0.6% 1556 kg/mm2 >1790 ◦ C
Mohs hardness of 8.5–9 and refractoriness higher than that of TFS. These cm3
characteristics make it highly suitable for reuse in refractory materials. TFS 3.28 g/ 9% 1080 kg/mm2 >1790 ◦ C
For large ferroalloy enterprises with a production history of more than cm3
Brown fused 3.81 g/ 5.4% 1800− 2200 kg/ >1790 ◦ C
several decades, ferrotitanium slags have accumulated in considerable
alumina cm3 mm2
amounts in dumping sites, and most of them are LFS [25]. The appli­
cation of LFS mainly focuses on the high TiO2 content in its chemical
composition for use as a sintering aid in aluminum–magnesium cast­
ables [26,27]. However, few studies have used LFS as the main raw
material. The characteristics and evaluation of LFS as main additive raw
material for refractory is of great significance in promoting the use of
LFS.
Owing to their low cost, sustainable materials show a great potential
in the raw material market; hence, refractory manufacturers pay sub­
stantial attention to their stability, i.e., product composition fluctua­
tions, and product stability in different application environments [18] In
this study, an electric arc furnace was used to prepare remelting
low-fluxing ferrotitanium slag (RLFS) for homogenization and impurity
removal. The properties and stability of RLFS as a refractory raw ma­
terial were characterized, and a phase-structure transition mechanism of
RLFS particles was established according to the thermal stability results
and thermodynamic calculations.

2. Experimental

2.1. Remelting process of LFS

Fig. 2. XRD pattern of RLFS.
The research samples used in this study were based on dumping slags

Fig. 1. Remelting process of dumping slags (LFS).

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Fig. 3. SEM-EDS images of RLFS.

Fig. 4. (a) Thermal conductivity, (b) coefficient of thermal expansion and linear expansion, and (c) TG-DSC results of RLFS.

Table 4 Table 5
Thermal conductivity of inorganic materials. Thermal conductivity of inorganic materials (W⋅m− 1⋅K− 1).
Adj. R-Square predicted data(W⋅m− 1⋅K− 1) 25 ◦ C 100 ◦ C 500 ◦ C 1000 ◦ C

1000 C ◦
1500 C ◦
1600 C ◦
Magnesia 40 35 16 7
Corundum 38 35 11 7
Exponential fit 0.99851 4.90 5.33 5.72
Mullite – 1.8 2 7
Polynomial fit 0.99833 4.41 2.98 2.79
Power fit 0.93909 6.25 5.68 5.60

molten state in an electric arc furnace and then kept at 2000–2200 ◦ C for
from low-fluxing ferrotitanium production smelting with ilmenite 3–5 h. While the LFS remained molten, metals settled to the bottom due
concentrate. The chemical composition of these dumping slags (LFS) is to gravity and bubbles floated up and escaped into the environment due
shown in Table 1. Due to limitations in the low-fluxing ferrotitanium to the buoyancy of the molten slag. Remelting products were obtained
production process, metal exists in the slag as the form of inclusions, after natural cooling.
resulting in the high content of TiO2 and Fe2O3 in chemical composition. The remelting products—which were divided into blocks and gran­
The remelting process is shown in Fig. 1, where LFS was heated to the ules after crushing—were used for this study as RLFS. The RLFS samples

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Fig. 5. Thermal stability test of RLFS samples.

Fig. 6. SEM images of the RLFS samples after heat treatment at 1200, 1500, and 1600 ◦ C.

used in this study were provided by Jinzhou Guotai Industrial Co., Ltd. sample was calculated according to the following formula: Hv =
0.1891*F/D2, where Hv is the Vickers hardness, F is the test force (N),
2.2. Characterization and D is the arithmetic mean of the two indentation diagonals (mm).
Analysis of the chemical composition was conducted using an IRIS
In this study, the bulk density and apparent porosity of the particle Advantage Radial inductively coupled optical plasma emission spec­
samples were measured according to the Archimedes principle, and the trometer (ICP-OES, ThermoElemental Instruments, USA). The refracto­
Vickers indentation method was used to measure the microhardness of riness was measured according to ISO 528:1983.
the samples. Surface polished samples were indented under a load of 50 The phase evolution was analyzed using X-ray diffraction (XRD;
kg, and the diagonal length of the indentation was measured from X’Pert Pro, Philips) with CuKα as the radiation source, a tube voltage of
scanning electron microscopy (SEM) images. The microhardness of the 40 kV, a tube current of 40 mA, and a continuous scanning rate of 2◦ /

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3.2. Phase and microstructure of RLFS

The XRD pattern of RLFS sample is shown in Fig. 2. The major

diffraction peaks were indexed as corundum (α-Al2O3; PDF# 75–0782)
and titanium oxide (Ti2O3; PDF# 71–1054). The SEM–EDS image of
RLFS sample in Fig. 3 shows that the sample has a structure composed of
two contrasting areas. According to the EDS results, the main elements
in the dark area were Al and O, and this area was identified as corundum
based on the XRD results. The main elements in the light area were Ti,
Al, and O. Based on the XRD results and literature [31], the main phases
in this area may be (Al,Ti)2O3 crystals formed with Al2O3 and Ti2O3.

3.3. Thermodynamic properties of RLFS

As shown in Fig. 4(a), thermal conductivity of RLFS was measured at

five temperature points (100, 200, 300, 400, and 500 ◦ C). The results
indicate that the thermal conductivity of the sample decreases with
increasing temperature. Polynomial, exponential and power fits were
used in trend prediction of the thermal conductivity at higher temper­
Fig. 7. XRD pattern of different feature areas in RLFS samples after ature. In third- or higher-order polynomial fitting, a negative value was
heat treatment. predicted; therefore, second-order polynomial fitting was used in this
study. A degree-of-freedom adjusted coefficient of determination (Adj.
min over a range of 10–90◦ . The microstructural evolution of the spec­ R-Square) of the various fitting function and the data predicted using the
imens was examined by SEM (JSM-6610, JEOL, Japan), and elemental various fitting functions are shown in Table 4. The exponential and
analysis was performed using energy dispersive X-ray spectroscopy polynomial fits have higher Adj. R-Square values than the power fit. The
(EDS, QUANTAX200-30, Bruker, Germany). thermal conductivity was predicted for several service temperatures of
A comprehensive thermal analyzer (STA449, NETZSCH, Germany) refractories, where the exponential and power fits gave similar values at
was used to obtain the thermogravimetric analysis (TG) and differential high service temperature(1500, 1600 ◦ C). In summary, the thermal
scanning calorimetry (DSC) curve of the RLFS sample; and a thermal conductivity predicted by polynomial fitting is of a certain significance.
dilatometer (DIL 402 Expedis Classic, NETZSCH, Germany) was used to The thermal conductivities of several refractory raw materials are
detect the thermal expansion coefficient and the change in the thermal listed in Table 5 [32]. This indicates that the thermal conductivity of the
expansion coefficient of the sample. RLFS samples were processed into RLFS sample is lower than that of corundum and magnesia, and that the
disks with a diameter of 12.5 mm and thickness of 2 mm, and the thermal insulation performance of RLFS at 1000 ◦ C is also better than
thermal conductivity was measured using a laser thermal conductivity that of traditional refractory raw materials. This means that the appli­
tester (Flashline-5000, Anter, USA). cation of RLFS as a refractory raw material is conducive for reducing the
thermal conductivity of refractory materials, improving the overall
3. Results and discussion insulation performance of the furnace lining, and reducing production
costs.
3.1. Physical and chemical properties The thermal expansion coefficient and linear expansion of the RLFS
are shown in Fig. 4(b). The average thermal expansion coefficient of the
The RLFS appeared as a black block after crushing (Fig. 1). The sample was approximately 8.8 × 10− 6/◦ C. This indicates that the ther­
chemical composition of RLFS is shown in Table 2. The main chemical mal expansion coefficient of RLFS is the same as to that of corundum
∑
components of RLFS are titanium oxide ( TiO2+Ti2O3+TiO + Ti) and (8.8 × 10− 6/◦ C), which shows that RLFS and corundum have good
alumina. The alumina content is above 80 wt%, which is higher than volume compatibility.
that in TFS (above 75 wt%) [23]. The RLFS sample increased in weight The DSC–TG results of RLFS heated from room temperature (20 ◦ C)
by approximately 1.16 wt% during the ignition loss test, which indicates to 1200 ◦ C in air are shown in Fig. 4(c). The sample showed a uniform
that the presence of titanium suboxide or metal inclusions in the slag weight gain and exothermic behavior throughout the process; the
increased the oxidative weight during the test. The physical properties of weight of sample increased by about 3.5% over the entire process. The
RLFS, TFS, and brown corundum are listed in Table 3 [28–30]. They DSC curve indicated that the structure of RLFS showed a transition tend
indicate that the bulk density and hardness of RLFS are higher than those to reach a more stable state of lower chaos during the heating process,
of TFS and close to those of brown corundum. perhaps due to the oxidation behavior of the titanium suboxide (Ti2O3)
in the sample.

Fig. 8. Phase-structure transition mechanism of RLFS particles under oxidizing conditions.

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3.4. Thermal stability and phase-structure transition mechanism of RLFS the TiO2 oxide layer. There was no evident cracks area observed in the
reactive layer, which indicates that the generation of the cracks area
To test the thermal stability of RLFS in different atmospheres, three does not occur from the outside to inside. The cracks area was generated
groups of RLFS samples were heat treated at 1600 ◦ C for 3 h in CO, later than the reactive layer. The formation temperature of the cracks
argon, and air. The samples heated in a CO or argon atmosphere retained area was lower than the initial temperature of reaction in Eq. (2). To
their original appearance, whereas those heated in air showed different keep the structural stability of RLFS, the formation of the reactive layer
colors on the surface (Fig. 5). Thermodynamic calculations of possible should be avoided; therefore, using RLFS in refractory products that
reactions were performed using Factsage™ 6.2 software (ESM Software, require an oxidizing working atmosphere with temperatures higher than
USA). According to the results of thermodynamic calculations, the re­ 1280 ◦ C should be avoided.
actions in Eqs (1) and (2) may occur in these samples when T > 402 K
(229 ◦ C), ΔG1<0, and when T > 1553 K (1280 ◦ C), ΔG2<0, respectively. 4. Conclusion
2Ti2 O3 + O2 →4TiO2 ΔGθ1 = 75255 − 187T(J / mol) (1)
The material characteristics of RLFS make it highly valuable for reuse
in high-alumina/corundum refractories. Its physical properties and
TiO2 + Al2 O3 →Al2 TiO5 ΔGθ2 = 17000 − 10.95T(J / mol) (2)
thermal expansion coefficient are close to those of corundum, and it has
Five groups of RLFS samples were heat treated in air for 3 h at 1200, lower thermal conductivity, which makes it suitable as a substitute for
1300, 1400, 1500 and 1600 ◦ C. After heat treatment, the samples were common corundum raw materials (such as brown corundum). Accord­
sectioned, and the thickness of the discolored area was found to have ing to the thermal stability test results and analysis of the phase-
increased with increasing heat treatment temperature. The discolored structure transition mechanism, using RLFS in refractory products that
area of the samples after heat treatment at 1200 ◦ C was found to be require an oxidizing working atmosphere with temperature higher than
limited to the surface layer. Evident cracks were observed on the surface 1280 ◦ C should be avoided. In addition, for refractory products that
of the samples after heat treatment at 1600 ◦ C. SEM–EDS image of the work under reducing conditions (such as blast furnaces, hot metal ladles,
sample treated at 1200 ◦ C is shown in Fig. 6(a). There were many ladle linings, and bottom bricks), RLFS has good application prospects
transverse cracks near the surface layer, whilst the internal area main­ because of its comprehensive performance compared to corundum ma­
tained the original dense structure. From the results of EDS mapping, Al terials. The resource treatment process of RLFS is generally the same as
and Ti aggregations in the RLFS had different distribution areas. This that of TFS, which indicates that manufacturers that process TFS recy­
indicates that the light contrast area is mainly dominated by Ti2O3 cled raw materials can use existing equipment to process RLFS without
crystals, with a small amount of Al doping. Fig. 6(b) and (c) show the additional equipment costs.
SEM images of the samples after heating to 1500 and 1600 ◦ C, respec­ The present work showcases the high potential of RLFS for applica­
tively. There were areas with transverse cracks observed after the tion in refractory products as raw material markets will need cheap and
sample was heated to 1500 ◦ C. When comparing samples heated at well-performing alternatives to manage the depletion of traditional raw
different temperatures, it was found that the cracked area was closer to materials. The physical and chemical properties, thermodynamic prop­
the bulk of the sample, and the light contrast area near the surface of the erties, and thermal stability of RLFS after resource treatment have been
sample was not observed and produces a gray contrast area with a loose analyzed and tested, and its application as a potential refractory raw
structure. In this paper, the area with such characteristics is called the material has been evaluated. The following conclusions can be drawn:
reactive area, the area with transverse cracks is called the cracks area,
and the area without change is called the original area. Fig. 6(c) shows (1) After resource treatment, RLFS exhibits a lower thermal con­
an SEM image of the junction between the reactive layer and the cracks ductivity than, and a thermal expansion coefficient similar to that
area in the sample after heat treatment at 1600 ◦ C. It is evident that there of brown corundum. RLFS can thus be used as a substitute for
were more connected pores in the gray contrast area of the reactive corundum in high-alumina refractories and corundum
layer, and the structure was significantly damaged. The thickness of the refractories.
reactive layer of this sample was significantly higher than that of the (2) RLFS undergoes drastic structural changes from the outside to the
sample heat treated at 1500 ◦ C. Fig. 7 shows XRD patterns sampled from inside under oxidation conditions with temperature above
the original area, the cracks area, and the reactive layer. The phase 1280 ◦ C. The use of RLFS particles in refractory materials that are
composition of the original area showed Ti2O3 and Al2O3 composition of subjected to such conditions should be avoided.
the as-prepared sample. The rutile (TiO2) phase was observed in the (3) RLFS has similar physical and chemical properties to and lower
cracks area, and the Ti2O3 phase was not observed at all in the reactive thermal conductivity than corundum materials, and its good
layer. The main phases were corundum and aluminum titanate, with a stability in a reducing atmosphere makes it suitable for ladle
small rutile phase, which is consistent with the thermodynamic calcu­ working linings and ladle bottom bricks.
lation results.
A phase-structure transition mechanism of RLFS particles under an
Declaration of competing interest
oxidizing atmosphere was established according to the thermal stability
results and thermodynamic calculations (Fig. 8). When the RLFS was
The authors declare that they have no known competing financial
heated above 229 ◦ C in air, reaction in Eq. (1) started in the oxide layer
interests or personal relationships that could have appeared to influence
to generate TiO2. However, the dense TiO2 oxide layer limited the
the work reported in this paper.
diffusion of the oxidation reaction to the inside of the sample, which
prevented the inside area from being oxidized. However, when heated
Acknowledgments
above 1280 ◦ C in air, reaction in Eq. (2) occurred in the oxide layer to
form the reactive layer, consuming the TiO2 generated in reaction in Eq.
This work was funded by the National Natural Science Foundation of
(1). Al2TiO5 generated in the Ti-rich area resulted in larger volume
China (NO.51804233).
shrinkage and many interconnected voids in the reactive layer, accel­
erating the oxidation reaction and extending it to the inside area. The
speed of the diffusion of the oxidation reaction increases with increasing References
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