Melt corrosion of refractories in the nonferrous industry and the electric arc furnace: A thermochemical approach*

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1 Pure Appl. Chem., Vol. 83, No. 5, pp , doi: /pac-con IUPAC, Publication date (Web): 4 April 2011 Melt corrosion of refractories in the nonferrous industry and the electric arc furnace: A thermochemical approach* Viktoria Reiter 1, and Harald Harmuth 2, 1 RHI AG, TCL Leoben, Magnesitstraße 2, 8700 Leoben, Austria; 2 University of Leoben, Peter-Tunner-Straße 5, 8700 Leoben, Austria Abstract: A thermochemical approach was implemented to study the dissolution mechanisms of a wide range of refractory oxides and silicates in slags of the nonferrous metals industry and electric arc furnaces. First of all, the slags have been characterized regarding their working range, phase assemblage, and melting behavior. Subsequently, the interactions of different combinations of refractory and slag have been examined, and emphasis has been placed on the determination of possible reaction products formed during dissolution and the solubilities of the refractory oxides and silicates in various slags. Direct dissolution, decisive in the case of high corrosion rates, as well as indirect dissolution have been described. Varying operation conditions (e.g., temperature, atmosphere) have been incorporated into the investigations. In addition to the thermochemical calculations, the solubility of magnesia in fayalite slags has been determined experimentally with the quenching method and the calculated results have been compared to published corrosion studies of other authors. These studies revealed that thermochemical calculations are a suitable tool to examine melt corrosion. The thermochemical approach provides information that can be incorporated into product development and in the operation mode, giving a proper choice of process conditions. Keywords: dissolution; melt corrosion; nonferrous metals; refractories; thermochemical calculations. INTRODUCTION In steel plants refractory costs account for approximately 2 3 % of total production costs. For example, in electric arc furnaces approximately 408 kg of refractories per 100 tons of steel are consumed. The refractory wear should be minimized to reduce costs and to increase productivity that is lost by new linings and repairs. To reduce refractory wear, emphasis must be placed not only on product development but also on the steel-making practice with regard to slag chemistry and service conditions. Refractories in metallurgical vessels must resist high temperatures, thermo-mechanical stresses (erosion, abrasion), and attack of corrosive atmospheres, hot metals, and slags (chemical wear). For ceramically bonded materials melt corrosion proceeds via penetration and dissolution [1]. The penetration depth depends on the pore structure of the refractory material and the viscosity, surface tension, and wetting angle of the slag. A thermal gradient prevails from the hot face to the cold end of the refractory lining. This results in fractional crystallization and freezing of the penetrated melt and thus a densifying of the *Paper based on a presentation made at the 14 th International Symposium on Solubility Phenomena and Related Equilibrium Processes (ISSP-14), Leoben, Austria, July Other presentations are published in this issue, pp Corresponding author: viktoria.reiter@rhi-ag.com harald.harmuth@unileoben.ac.at 1093

2 1094 V. REITER AND H. HARMUTH microstructure. The dissolution process may be direct or indirect. Indirect dissolution comprises the formation of one or more reaction products at the refractory/slag interface that may act as a protective layer. However, in the case of high corrosion rates assuming a high erosion rate due to bath agitation direct dissolution will prevail. First of all, the bonding phases and the matrix will be dissolved, resulting in a loss of bond that in turn favors the erosion of grains. This assumption is based on postmortem investigations of used refractory samples. In the case of diffusion-controlled dissolution the corrosion rate essentially depends on the ion flux j which may be expressed according to Fick s First Law [2] (1). D j = c (1) S c δ ( 0 ) The ion flux j is defined by the effective diffusion coefficient (D), the effective thickness of the boundary layer (Nernst) (δ), the saturation concentration (c S ), and the concentration of the component in the slag (c 0 ). The solubility limit is an important parameter in the dissolution process, e.g., slags saturated in MgO decrease MgO dissolution. A first approach to rank refractory components with respect to their resistance against slag attack is to compare their solubility limits. Refractory consumption can be reduced by a proper choice of the refractory depending on slag chemistry in order to minimize the concentration difference (c S c 0 ). For many decades phase diagrams have been used successfully to evaluate solubilities and phase equilibria in refractory corrosion [3]. Nowadays, self-consistent thermo - chemical databases are so advanced that computational thermodynamics can be applied successfully to multicomponent phase equilibria. This study has put emphasis on thermodynamic modeling of dissolution mechanisms (direct and indirect) of refractory material components in slags of the nonferrous industry and electric arc furnace slags. Thermochemically self-consistent databases are fundamental for accurate and reliable predictions. The thermodynamic calculations have been performed with the software package FactSage as the FactData have been proven to be one of the best optimized commercially available data sets for oxide systems. The Gibbs energy minimization modules Equilib and Phase Diagram have been used in combination with the FACT53, FToxid, and FTmisc databases. Proposals for possible improvements in the field of process performance, lining design, product selection, and product development are provided in order to decrease refractory wear and increase service life. THERMOCHEMICAL MODELING AND EXPERIMENTAL PROCEDURE Figure 1 represents schematically the approach for the thermochemical modeling of the corrosion mechanisms. Fig. 1 Schematic representation of the applied methodology.

3 Melt corrosion of refractories 1095 As the slag is the attacking medium and its characteristics have a crucial influence on the corrosion, first the working range of the slags and their phase constitution have been described in detail. Afterwards, the refractory/slag equilibria have been determined for direct and indirect dissolution. The investigated materials comprise the main phases (oxides and silicates) of basic and nonbasic refractory materials (see Table 1). The dissolution behavior of the refractory material has been characterized with the following parameters: (a) reaction products occurring at the solid/liquid interface including their compositions, (b) solubility limits, and (c) amount of refractory material dissolved in 100 g slag. Table 1 Investigated refractory oxides and silicates. Oxides Silicates MgO Mg 2 SiO 4 Al 2 O 3 CaMgSiO 4 Cr 2 O 3 Ca 3 MgSi 2 O 8 ZrO 2 Ca 2 SiO 4 MgCr 2 O 4 MgAl 2 O 4 The calculations have been adapted to several service conditions by varying temperature (gradient from the hot face to the cold end), atmosphere (oxygen partial pressure), refractory/slag ratio, and local slag composition. The calculated results have been evaluated by comparison with published results of corrosion studies by other authors. These studies comprise microanalytical investigations of refractories after crucible tests. Indirect dissolution was observed as reaction products have been formed at the refractory/slag interface [4,5]. Additionally, the solubility of MgO has been determined experimentally in fayalite slags with the quenching method. Mixtures of MgO and fayalite slag with increasing refractory/slag ratios have been equilibrated in air at 1550 C. Subsequently, the samples have been quenched in water to freeze the phase assemblage at test temperature and if possible to solidify the residual melt in a glassy state. The phase constitution and the compositions of the phases have been determined with microscopy and microanalytical methods and have been compared to calculated results. Slags of the nonferrous metals industry Copper-converting slags can be classified with respect to the process technology as fayalite slags (discontinuous process, e.g., Peirce Smith converter) and calcium ferrite slags (continuous converting, e.g., Mitsubishi process). However, these slags have several drawbacks. Fayalite slags are characterized by high viscosity and a high risk of magnetite precipitation, while calcium ferrite slags show a low solubility for SiO 2 and are very corrosive. The newly proposed ferrous calcium silicate (FCS) slags should avoid these drawbacks and combine the advantages of fayalite and calcium ferrite slags [5,6]. In the copper converter a magnesiachromite lining is common practice as it shows the highest resistance against the mostly used fayalite slags. Nevertheless, there are attempts to replace magnesiachromite because of the possible formation of harmful hexavalent chromium. The investigations should point out from a thermochemical point of view which refractory materials could be taken into account as replacements for magnesiachromite and how the slag chemistry influences dissolution behavior (calcium ferrite, fayalite, and FCS slags). The refractory components will be ranked with rising corrosion resistance. Furthermore, the advantages of FCS slags with regard to lower dissolution rates are pointed out since there is limited data regarding the wear behavior of FCS slags.

4 1096 V. REITER AND H. HARMUTH Corrosion environment Four fayalite slags (1 4), one calcium ferrite slag (5), and one FCS slag (6) have been incorporated in the investigations (see Table 2). The fayalite slags 1 3 and the calcium ferrite slag are converter slags of different copper mills, slag 4 represents a synthetic fayalite slag. The composition of the FCS slag has been chosen to assure that the slag is completely liquid at process temperature and lies in the vicinity of the primary phase field of dicalcium silicate. Table 2 Chemical composition of the investigated slags. [wt %] Fe 2 O SiO CaO MgO Al 2 O Cu 2 O ZnO PbO The main components of the slags of the nonferrous metals industry are CaO, SiO 2, and FeO x. The molar ratio Fe/SiO 2 of the fayalite slags ranges from 1.3 to The FCS slag has a basicity, expressed by the molar ratio CaO/SiO 2, of 1. Processes working with fayalite slags necessitate an oxygen partial pressure (po 2 ) of atm to avoid magnetite precipitation; in the case of calcium ferrite slags, the po 2 may rise to 10 5 atm. Slag characterization The working range of the slags of the nonferrous metals industry is mainly defined by the liquidus surfaces in the three-component system CaO SiO 2 FeO x that are shown in relation to the oxygen partial pressure in Fig. 2. Additionally, the compositions of the investigated slags are inserted. The working range of calcium ferrite slags is determined by the liquidus area at the base line of the triangle. The second liquidus area that is relevant for fayalite and FCS slags decreases in size with increasing oxygen partial pressure. Besides the main components, other oxides have to be considered as the liquid domain is enlarged by Al 2 O 3, ZnO, PbO, and Cu 2 O and diminished by MgO. The valency of iron strongly affects the phase composition and the melting behavior of the slags. Olivine with inclusions of MgO, CaO, and ZnO is the main phase of fayalite slags under reducing conditions. With increasing oxygen partial pressure the ratio Fe 2+ /Fe 3+ decreases and the phase composition shifts toward spinel related to magnetite. The copper-containing phase changes with decreasing po 2 from cuprospinel (CuFe 2 O 4 ) to delafossite (Cu 2 Fe 2 O 4 ) and finally to metallic copper. The main phases of calcium ferrite slags are dicalcium ferrite, calcium ferrite, and a copper-containing phase that depends again on the prevailing oxygen partial pressure. The phase composition of the FCS slag is similar to the fayalite slag, but wollastonite or rankinite are also stable.

5 Melt corrosion of refractories 1097 Fig. 2 Liquid domain in the CaO SiO 2 FeO x system at 1250 C in relation to oxygen partial pressure. Thermochemical modeling of refractory/slag equilibria Indirect dissolution: The reaction products that may be formed at the refractory/slag interface are summarized in Table 3; however, the levels were dependent on the specific slag/refractory component ratio. The investigations yield the following results for the dissolution of MgO: attack of MgO by fayalite slags results in a complete dissolution of MgO at low MgO/slag ratios, followed by the formation of olivine, magnesiowustite, and spinel with rising MgO/slag ratios. Zirconia does not form any reaction products in combination with the iron silicate and FCS slags, whereas CaZrO 3 was formed with the calcium ferrite slag. Table 3 Potential reaction products at the refractory/slag interface. Abbreviations are CaAl 4 O 7 (CA 2 ), CaAl 12 O 19 (CA 6 ), and Ca 2 SiO 4 (C 2 S). Fayalite slag Refractory Calcium ferrite slag Spinel, cristobalite, eskolaite Cr 2 O 3 Spinel, C 2 S, CaCr 2 O 4, eskolaite Olivine, spinel, magnesiowustite MgO Spinel, magnesiowustite Spinel, corundum Al 2 O 3 Spinel, melilite, CA 2, CA 6, corundum Zirconia ZrO 2 CaZrO 3, zirconia Olivine, spinel MgCr 2 O 4 Spinel, C 2 S, CaCr 2 O 4 Olivine, spinel MgAl 2 O 4 Melilite, spinel The amount of dissolved refractory material in 100 g slag is shown for indirect dissolution in Fig. 3.

6 1098 V. REITER AND H. HARMUTH Fig. 3 Amount of refractory oxides dissolved in 100 g slag at 1250 C and for indirect dissolution. Cr 2 O 3 and MgCr 2 O 4 exhibit the lowest solubility, nearly independent of slag composition due to the formation of an iron-containing spinel. The amount of dissolved magnesia is 1 3 g. Zirconia shows a lower solubility in the calcium ferrite and FCS slags due to the formation of CaZrO 3. In fayalite slags no reaction products are formed and the solubility of ZrO 2 decreases with decreasing Fe/SiO 2 ratio. The solubility of alumina increases with rising CaO content of the slags and is highest for the calcium ferrite slag. The solubility limits of the refractory components decrease with decreasing temperature and oxygen partial pressure linearly with the logarithm of oxygen partial pressure. MgO and Cr 2 O 3 solubility increases 1 2 wt %/100 C, whereas the solubility of Al 2 O 3 increases 5 wt %/100 C. Silicate solubilities in iron silicate slags increase from forsterite (Mg 2 SiO 4 ) to monticellite (CaMgSiO 4 ) to merwinite (Ca 3 MgSi 2 O 8 ) to dicalcium silicate (Ca 2 SiO 4 ) (see Fig. 4). In calcium ferrite and FCS slags the various silicate solubilities are of the same order of magnitude. Additionally, the silicate solubilities are considerably lower in these slags compared to the iron silicate slags due to the high initial CaO content in the calcium ferrite and FCS slags. Fig. 4 Amount of silicates dissolved in 100 g slag at 1250 C and for indirect dissolution. Abbreviations are Ca 2 SiO 4 (C 2 S), Ca 3 MgSi 2 O 8 (C 3 MS 2 ), CaMgSiO 4 (CMS), and Mg 2 SiO 4 (M 2 S). Direct dissolution: The calculated refractory oxide solubilities in all the slags were higher for direct dissolution compared to indirect dissolution (Fig. 5). Cr 2 O 3 and MgCr 2 O 4 solubilities were the lowest compared to the other oxides in the iron silicate and FCS slags; however, in the calcium ferrite slag they were higher relative to MgO and ZrO 2. The solubilities of Cr 2 O 3, MgCr 2 O 4, and MgO decreased with increasing slag basicity, namely, the solubilities were lower in the FCS slag. Therefore, the use of FCS slags should be favored in combination with refractory products based on these oxides. The solubility of alumina increased in the FCS slag due to its dependence on the CaO content of the slag. Slag 2 shows a high initial Al 2 O 3 content, and thus the solubilities of Al 2 O 3 and MgAl 2 O 4 are lower compared to other fayalite slags.

7 Melt corrosion of refractories 1099 Fig. 5 Amount of refractory oxides dissolved in 100 g slag at 1250 C and for direct dissolution. Silicate solubilities in the slags are illustrated in Fig. 6. As determined for indirect dissolution, the solubility of forsterite was significantly lower in the iron silicate slags compared to the CaO-containing silicates. The silicates showed considerably higher solubilities than the refractory oxides. The dissolution of these silicates results in bonding loss, weakening the refractory microstructure and enhancing erosive wear. Once again, the FCS slag demonstrated lower silicate solubilities compared to the iron silicate slags. Fig. 6 Amount of silicates dissolved in 100 g slag at 1250 C and for direct dissolution. In fayalite and FCS slags the solubilities of the oxides can be ranked with increasing solubility: Cr 2 O 3, MgCr 2 O 4, ZrO 2, Al 2 O 3, and MgO. The higher basicity of FCS slags leads to a lower solubility compared to fayalite slags. FCS may therefore lead to higher corrosion resistance or they may contribute to a chrome-free lining. It has been shown that besides proper product selection the process conditions, especially the slag composition, have a crucial influence on refractory wear. Refractory wear also depends considerably on the temperature and oxygen partial pressure. Thus, process control with regard to constant conditions also plays an important role. Evaluation of corrosion studies Experimental determination of the solubility of MgO in fayalite slags: The calculated and experimentally determined phase composition of the magnesia/slag 4 equilibria is shown in Fig. 7. Here, <A> denotes the mass percentage of magnesia relative to the sum of magnesia plus slag. The reaction products formed are spinel, olivine, and magnesiowustite. The homogeneous composition of the phases indicates that equilibrium has been reached in the experiments.

8 1100 V. REITER AND H. HARMUTH Fig. 7 Experimentally determined and calculated phase composition of the magnesia/slag 4 equilibria in air at 1550 C. The experimentally determined amount of spinel is higher compared to the calculations up to <A> = 25 wt %, resulting in a lower amount of liquid. In the mixtures, magnesiowustite is not stable until <A> = 40 wt % and so the amount of olivine is considerably higher. The cooling rate was too low to freeze the liquid completely glassy, i.e., magnetite, olivine, and a residual glass phase formed from the melt during cooling. These phases can be distinguished from the reaction products formed at 1550 C due to their morphology, and the area that represents the former melt at 1550 C can be defined explicitly. The experimentally determined and calculated compositions of spinel, olivine, and the residual melt are shown in Fig. 8 in relation to <A>. The calculated and experimentally determined compositions of olivine agree well, whereas the spinel has a higher magnesia and a lower iron content compared with the calculations. The residual melt shows a higher SiO 2 and a lower Fe 2 O 3 and MgO content as calculated. This deviation arises from the higher amount of spinel, whereby a higher amount of iron from the slag has reacted to spinel leading to an enrichment of SiO 2 in the residual melt. Additionally, the magnesia content of the spinel in the quenching tests is higher compared to the calculation leading to a lower amount of dissolved magnesia. The results of the calculations and the quenching tests agree well with respect to the qualitative phase assemblage and the composition of the reaction products. Tolerable differences exist in the quantitative phase composition and the composition of the residual melt. Therefore, this method can be used to evaluate the calculated results as well as to determine the solubility of oxides for which no adequate thermochemical data are available.

9 Melt corrosion of refractories 1101 Fig. 8 Experimentally determined and calculated compositions of the phases in air at 1550 C: (a) spinel, (b) olivine, and (c) residual melt. The solid lines and points represent the results of the calculations and the quenching tests, respectively. Corrosion studies of other authors: The investigated reaction products formed at the refractory/slag interface as well as the solubilities of magnesia and Cr 2 O 3 agree well with the results of the thermochemical calculations (see Table 4). However, the solubility of alumina in calcium ferrite slags is lower than in the calculations due to the different CaO content of the slags used in the corrosion studies and the calculations. Table 4 Solubilities [wt%] of MgO, Al 2 O 3, and Cr 2 O 3. Fayalite Calcium ferrite Calc. Lit. Calc. Lit. MgO [4] Al 2 O Cr 2 O [4] [6]

10 1102 V. REITER AND H. HARMUTH Electric arc furnace slag The main refractory materials used in the slag line of electric arc furnaces are carbon-containing bricks (MgO C bricks) and a MgO-based repair mix [7]. The influence of the dissolution rate on the slag composition (basicity), temperature, and oxygen partial pressure is discussed below. Corrosion environment Six slags (medium attacking) from three different electric steel plants were characterized. The three plants were chosen to cover a wide range of steel-making practices (see Table 5). Table 5 Chemical composition of electric arc furnace (EAF) slags. [wt %] A-I A-II B-I B-II C-I C-II CaO SiO Fe 2 O Al 2 O MgO MnO C/S The chemical compositions of slags A represent average analyses, whereas the slags of client B and C were sampled after tapping. EAF slags typically contain six major oxides (CaO, MgO, SiO 2, FeO, MnO, Al 2 O 3 ). The basicity (C/S ratio) ranges from 1.41 to This is an indicator of the different methods of EAF refining in steel plants [7]. Thermochemical modeling of refractory/slag equilibria Thermochemical modeling of MgO/slag interactions revealed refractory brick, and mix dissolution is controlled by the diffusion of FeO and MnO into the magnesia and the formation of a magnesiowuestite boundary layer. The formation of a solid reaction product at the refractory/slag interface indicated a diffusion-controlled indirect dissolution process. The solubility limit of MgO and the resulting concentration difference as considered in eq. 1 are shown in Fig. 9. Fig. 9 Solubility limit of MgO at 1650 C and log po 2 = 9. The solubility limit of MgO ranges from 4.4 to 12.6 wt %. These values agree well with published solubility limits [8,9]. The negative concentration difference of MgO for slags C-I and C-II reveals saturation in MgO. Plant C uses a slag conditioner providing MgO. No further dissolution of the refrac-

11 Melt corrosion of refractories 1103 tory material will take place except for the silicates. Whilst MgO refractories are severely attacked by unsaturated slags, in the case of saturated slags the oxidation resistance of carbon in MgO C refractories becomes the dominant factor affecting corrosion resistance. The impact of basicity and temperature on the solubility limit of magnesia is shown in Figs. 10a,b. A decrease in slag CaO/SiO 2 increased the MgO solubility, and dissolution of MgO would be accelerated. These results indicated highly basic slags would be less corrosive toward MgO grains. A temperature rise of 100 C resulted in a c S increase of wt %. With one exception the results showed a trend of higher MgO solubility with increasing oxygen partial pressure. Since trivalent iron is less basic than the bivalent form, the basic magnesia is less stable against Fe 3+ resulting in higher solubility limits at increased oxygen partial pressures. Additionally, the FeO MgO system is completely miscible, whereas the Fe 2 O 3 MgO system shows a miscibility gap. A change of the operation mode, especially the slag basicity, can be recommended to client A to reduce refractory corrosion. A C/S-ratio similar to client B and C should be strived for. Fig. 10 (a) Solubility limit of MgO in relation to basicity at 1650 C and log po 2 = 9; (b) solubility limit of MgO in relation to temperature at log po 2 = 9. CONCLUSION In the present study, it has been shown that thermochemical calculations are suitable to qualitatively examine melt corrosion. The output of the calculations can be incorporated into product development and the operation mode. They can be used to make predictions regarding the dissolution levels of refractory materials that may help to reduce costly experimental investigations. The study demonstrates that the dissolution rate of refractory components is significantly influenced by slag composition. For example, the use of FCS slags in the nonferrous metallurgy may reduce the dissolution rate of refractories

12 1104 V. REITER AND H. HARMUTH based on magnesia and magnesiochromite compared to fayalite slags. However, whilst it is important to consider the impact on refractory dissolution, the primary slag selection criteria are based on metallurgical process requirements. Good agreement between the calculated results and the experimentally determined phase compositions indicates that thermodynamic modeling is an appropriate method to determine refractory dissolution mechanisms in metallurgical slags. The calculations supply reliable results. So far there have been no attempts to incorporate the actual conditions of corrosion occurring in metallurgical vessels, for example, fluid flow, thermo-mechanical stresses, diffusion, and mass transport. To get a comprehensive model of refractory wear, thermochemical and thermomechanical considerations as well as computational fluid dynamics (CFD) calculations (mass transfer coefficients) must be combined. So far the simulation of subprocesses enables a better understanding of erosive and corrosive wear. For example, CFD can be used to calculate the mass transfer coefficient and in combination with the concentration difference the dissolution rate can be calculated. The thermomechanical wear, the crack formation, and joint opening that support the slag penetration and the melt corrosion can be described with finite element methods. Additional process simulation tools should be applied to determine the temperature, atmosphere, and local slag compositions in various metallurgical processes as exactly as possible. A challenge for the future is to link different simulation methods for a comprehensive description of corrosion, qualitatively as well as quantitatively. REFERENCES 1. W. E. Lee, S. Zhang. Int. Mater. Rev. 44, 77 (1999). 2. W. E. Lee, S. Zhang. Int. Mater. Rev. 45, 41 (2000). 3. W. E. Lee, B. B. Argent, S. Zhang. J. Am. Ceram. Soc. 85, 2911 (2002). 4. J. R. Donald, J. M. Toguri, C. Doyle. Metall. Mater. Trans. B 29, 317 (1998). 5. N. P. Fahey, D. R. Swinbourne, S. Yan, J. M. Osborne. Metall. Mater. Trans. B 35, 197 (2001). 6. A. Vartiainen, M. Kytö. Scand. J. Metall. 31, 298 (2002). 7. Y. Hoshiyama, Y. Ishihara. J. Tech. Ass. Refr. 21, 247 (2001). 8. S. Zhang, H. Sarpoolaky, N. J. Marriott, W. E. Lee. Br. Ceram. Trans. 99, 248 (2000). 9. A. Sander, F. Verhaeghe, B. Blanpain, P. Wollants, R. Hendricks, G. A. Heylen. Steel Res. Int. 77, 317 (2006).

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