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Xue-liang Zhang, Shu-feng Yang, Jing-she Li, and Jin-qiang Wu, Temperature-dependent evolution of oxide inclusions during heat treatment of stainless steel with yttrium addition, Int. J. Miner. Metall. Mater., 27(2020), No. 6, pp.754-763. https://dx.doi.org/10.1007/s12613-019-1935-1
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The evolution of oxide inclusions during isothermal heating of 18Cr–8Ni stainless steel with yttrium addition at temperatures of 1273 to 1573 K was investigated systematically. Homogeneous spherical Al–Y–Si(–Mn–Cr) oxide inclusions were observed in as-cast steel. After heating, most of the homogeneous inclusions were transformed into heterogeneous inclusions with Y-rich and Al-rich parts, even though some homogeneous oxide particles were still observed at 1273 and 1573 K. With the increase in heating temperature, more large-sized inclusions were formed. The shape of the inclusions also changed from spherical to irregular. The maximum transformation temperature of inclusions was determined to be 1373 K. The evolution mechanism of inclusions during heating was proposed to be the combined effect of the (i) internal transformation of inclusions due to the crystallization of glassy oxide and (ii) interfacial reaction between inclusions and steel matrix. Meanwhile, the internal transformation of inclusions was considered to be the main factor at heating temperatures less than 1473 K.
Precise control of non-metallic inclusions in steel is important because of the close relationship between steel quality and the characteristics of inclusions. Generally, inclusions with high melting point and high hardness can significantly decrease the strength, toughness, and fatigue resistance of steel products [1–6]. Rare earth metals (REM), such as cerium, yttrium, and lanthanum, have strong thermodynamic affinities with oxygen and sulfur, and are widely used to modify harmful inclusions and deeply purify steel [7–9]. Previous studies reported that the appropriate addition of REM to steel can effectively achieve the modification of inclusions and improve the performance of steel [10–14].
In previous studies, the behavior of inclusions in molten steel with REM addition had been extensively investigated [15–20]. Katsumata and Todoroki [15] analyzed the effect of cerium and aluminum on the characteristics of inclusions in 25Cr–8Ni stainless steel at 1873 K. Compared with Al killed steel, 25Cr–8Ni stainless steel exhibited lower deoxidation rate and higher oxygen content after Al–Ce complex deoxidation. A similar result was also observed in Al–Y killed steel [16]. The possible reason for this finding was the reduced flotation of Al–Ce–O inclusions from the melt because of the higher density of inclusions containing REM than inclusions containing Al2O3. Li et al. [17–18] investigated the evolution of inclusions in heat-resistant steel with Ce addition at 1873 K and during cooling. The Al–Si–O complex inclusions were observed at 60 min after deoxidation by Si–Al. However, after Ce addition, the Al–Si–O complex inclusions successively changed to Ce2O3 and inhomogeneous Ce–Al–Si–O inclusions with Ce2O3 core. Furthermore, the layered inclusions became homogeneous Ce–Al–Si–O particles during cooling. First, liquid Al–Si–O formed on the surface of Ce2O3 particles because of the presence of transition elements. Then, the solid Ce2O3 core melted and diffused into the shell during the solidification stage. Researchers [19–20] investigated the formation and growth mechanisms of REM (Ce, La, Pr, and Nd)–oxide cluster in 253MA stainless steel using the electrolytic extraction method. They determined that the cluster formed in liquid steel because of the effect of Brownian and turbulent collisions and grew by collision with individual inclusions. With the increase in the size of clusters, the large-sized cluster (circularity factor <0.15) tended to grow by collision with other clusters.
The formation, growth, and removal of rare earth oxide inclusions in molten steel and during the solidification stage have been well investigated. However, less attention has been focused on the evolution behavior of such inclusions in solid stainless steel. Recently, considerable research on the evolution behavior of oxide and sulfide inclusions in solid stainless steel during isothermal heating has been conducted [21–28]. Several researchers reported that MnO–SiO2 oxide inclusions in 18Cr–8Ni stainless steel changed to finer MnO–Cr2O3 oxide after heating at 1473 K because of the solid-state reaction between oxide inclusions and steel matrix [21–24]. Homogeneous Al–Ti oxide in Fe–Al–Ti alloy was transformed into heterogeneous Al–Ti oxide with Al-rich and Ti-rich parts because of the crystallization of glassy oxide during heating at 1573 K [25–26]. In addition, the evolution of MnS inclusions in Mg-treated E36 steel during heating at 1473 K was investigated by Wang and colleagues [27–28]. The individual MnS agglomerated and segregated on the surface of Al–Mg–Ti oxide inclusions after heating, which significantly promoted the formation of acicular ferrites in steel.
Yttrium addition to stainless steel has been considered in recent years because of its deoxidizing and desulfurizing effects; moreover, it improves the high-temperature oxidation resistance of materials [29–30]. Generally, slab reheating is necessary before hot rolling in stainless steel processing; thus, understanding the possible evolution of inclusions in this stage is important for the precise control of inclusions. However, to the authors’ knowledge, only a few studies focused on the evolution of such rare earth oxide inclusions during heating. Therefore, the present work aims to analyze the effect of isothermal heating at different temperatures on the evolution of yttrium-based oxide inclusions in solid stainless steel.
The chemical composition of as-cast stainless steel with yttrium addition is shown in Table 1. The as-cast stainless steel was prepared in an electric resistance furnace at 1873 K by carrying out the following procedures: First, 180 g of as-received 304 stainless steel billet was melted in an Al2O3 crucible (internal diameter of 35 mm and height of 70 mm) placed in the electric resistance furnace. Then, high-purity argon (>99.999%, flow rate of 0.3 m3/h) was introduced during the melting process. After isothermal holding at 1873 K for 15 min, 0.02 g yttrium ferroalloy (35wt%Fe–65wt%Y) wrapped in iron foil was added to the melt and stirred for approximately 10 s using a molybdenum bar to obtain a uniform composition of liquid steel. After deoxidation for 10 min, the melt was taken out and quenched by ice water. Inductively coupled plasma optical emission spectrometry and inert gas fusion impulse infrared absorption spectroscopy were employed to determine the contents of Si, Mn, Al, Y, and total oxygen.
| Fe | Cr | Ni | Si | Mn | Total Al | Y | Total O |
| Bal. | 18 | 8 | 0.38 | 1.55 | 0.006 | 0.0085 | 0.011 |
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Rectangular specimens (15 mm × 10 mm × 5 mm) were machined from the as-cast ingots for the subsequent heat treatment. To investigate the effect of heating temperature on the evolution of yttrium-based oxide inclusions, the steel specimens were placed in an electric resistance furnace. Within 0.5 min, the temperature of the furnace was increased to the target values. Then, the steel specimens were heat treated for 30 min in the range of 1273 to 1573 K. During isothermal heating, high-purity argon stream (>99.999%, flow rate of 0.2 m3/h) was introduced to prevent the oxidation of the heated samples. The deviation of heating temperature was controlled to be less than ±5 K during the entire heating process. After heating, the samples were taken out quickly and quenched by water.
The as-cast and heated steel samples were mounted in resin, ground with SiC paper, and mirror polished up to 0.25 µm by diamond suspension. To analyze the evolution of non-metallic inclusions during heating, at least 50 oxide inclusions were characterized in each sample using a scanning electron microscope equipped with an energy-dispersive spectrometer (SEM–EDS, Phenom ProX, Holland). At the same time, 45 electron microscopy images were taken from each specimen under ×1800 magnification, and the size distribution of inclusions in 0.99 mm2 was analyzed using the Image Pro 6.0 software. In this study, only the inclusions with diameters larger than 1 µm were counted and analyzed.
Fig. 1 shows the typical oxide inclusions in as-cast steel. Notably, the inclusions were homogeneous spherical Al–Y–Si(–Mn–Cr) oxide inclusions before heating. The size of most inclusions was less than 3.0 µm, which is similar to that observed in cerium-treated steel [15]. These homogeneous inclusions are also called “dark inclusions” in this study. The atomic concentrations of Al, Y, Si, Mn, Cr, and O in inclusions were determined by energy-dispersive spectroscopy. Al, Y, Si, Mn, and Cr were considered to exist as Al2O3, Y2O3, SiO2, MnO, and Cr2O3 in the oxide inclusions, respectively. On the basis of the conservation of the atoms of active metals, the composition of oxide inclusions was calculated. Approximately 50 inclusions were analyzed, and the composition of the inclusions was plotted on the Y2O3–Al2O3–(SiO2 + MnO + Cr2O3) ternary diagram, as shown in Fig. 2. The average composition of inclusions in as-cast steel was determined to be 20%Y2O3–34%Al2O3–27%SiO2–13%MnO–6%Cr2O3 (molar fraction). The average Y/Al molar ratio of the initial oxide inclusions was 0.58.
The oxide inclusions in heated steels were characterized, and the typical morphology and composition of inclusions are shown in Fig. 3. Complex oxide inclusions consisting of two phases were observed in the sample heated at 1273 K (Fig. 3(a)). A new gray phase with high yttrium content precipitated on the surface of the dark inclusions during heating and resulted in the transformation of inclusions from homogeneous to heterogeneous. Meanwhile, no significant change in the composition of the inclusion core compared with the homogeneous inclusions in as-cast steel was observed. In addition, some homogeneous oxide inclusions were observed after heating at 1273 K, as shown in Fig. 3(b). Both of the two types of inclusions were spherical.
With the increase in heating temperature to 1373, 1473, and 1573 K, more gray phases were observed in the inclusions and only a few residual dark phases were detected on the edge of the inclusions (Figs. 3(c), 3(d), and 3(e)). The shape of the inclusions also changed from spherical to irregular. Moreover, some homogeneous irregular inclusions were observed in the sample heated at 1573 K (Fig. 3(f)). These inclusions had lower SiO2 content but higher Cr2O3 content than the original inclusions in as-cast steel. Interfacial reaction between Cr in the steel matrix and SiO2 in the inclusions may have occurred and caused the transformation from MnO–SiO2-type inclusions into MnO–Cr2O3-type oxide. This finding is consistent with that observed in previous studies [21–22].
Fig. 4 illustrates the change in the fraction of homogeneous and heterogeneous inclusions in steels during heat treatment. The fraction of homogeneous oxide inclusions decreased from 100% to 42% after heating at 1273 K because of the precipitation of the new gray phase with high yttrium content on the surface of inclusions. With the increase in heating temperature to 1373 K, the fraction of homogeneous inclusions gradually decreased to zero and all of the inclusions changed to heterogeneous inclusions. However, approximately 40% of the inclusions in the sample heated at 1573 K still remained homogeneous. This finding indicates that the formation of heterogeneous particles was restricted at low or high heating temperatures.
To obtain more detailed information about the oxide inclusions in heated steels, mapping analysis of the typically heterogeneous oxide inclusions was performed, and the results are shown in Fig. 5. Notably, the gray phase of the inclusion corresponded to the Y-rich phase and the dark phase of the inclusion corresponded to the Al-rich phase. Line scanning was also conducted, and the results are shown in Fig. 6. O, Al, Y, and Si concentration gradients existing within the gray phase (Y-rich part) of the inclusion with a width of approximately 0.8 µm were clearly observed.
Fig. 7 shows the composition of oxide inclusions in steels heated at different temperatures. After heating at 1273 K, the composition of inclusions changed slightly, as shown in Fig. 7(a). The average Y/Al molar ratio of inclusions changed from 0.58 of the initial inclusions to 0.82 in the gray phase and 0.55 in the dark phase. With the increase in heating temperature to 1373 K, the homogeneous oxide inclusions in as-cast steel were significantly transformed into heterogeneous oxide inclusions with gray and dark phases, as shown in Fig. 7(b). The average Y/Al molar ratio in the gray phase considerably increased to 1.59, resulting in the formation of the Y-rich part in inclusions. At the same time, the Y/Al molar ratio in the dark phase decreased to 0.29, resulting in the formation of the Al-rich part in inclusions. When the heating temperature was increased to 1473 and 1573 K, as shown in Figs. 7(c) and 7(d), a change in inclusion composition was also clearly observed. However, the transformation of inclusions was actually not induced by the increase in temperature.
Fig. 8 illustrates the change in the average composition of different phases (i.e., gray and dark phases) in oxide inclusions with the heating temperature. The Al2O3 content in original inclusions decreased after heating, as shown in Fig. 8(a), whereas the Y2O3 and SiO2 contents in inclusions increased, which resulted in the formation of the gray phase in inclusions. With the increase in heating temperature from 1273 to 1573 K, the transformation of oxide inclusions was initially stimulated and subsequently inhibited. The most significant transformation of inclusions was observed at 1373 K. Fig. 8(b) shows the analysis results of the residual dark phase in inclusions. The composition of the residual dark phase in inclusions was retained after heating at 1273 K, whereas the composition of the dark phase in inclusions was obviously changed after isothermal holding at 1373 K. The Y2O3 and SiO2 contents of the dark phase in inclusions decreased significantly, whereas the Al2O3, MnO, and Cr2O3 contents increased. With the continuous increase in heating temperature, the composition of the dark phase in inclusions did not obviously change.
The size distribution and area fraction of yttrium-based oxide inclusions in as-cast and heated steels are presented in Fig. 9. Notably, most of the inclusions in as-cast steel were smaller than 3.0 µm. The area fractions of inclusions in as-cast steels with diameters of 1.0–1.5 and 1.5–2.0 µm were approximately 61% and 26%, respectively. After heat treatment, the fraction of small inclusions at 1473 K (diameter of 1.0–1.5 µm) decreased to approximately 52%, whereas that of inclusions larger than 2.0 µm obviously increased. With the increase in heating temperature, more large-sized inclusions were formed. As illustrated in Fig. 9(b), the area fraction of inclusions in steel gradually increased from 0.037% to approximately 0.05% after heating at different temperatures.
The homogeneous spherical Al–Y–Si(–Mn–Cr) oxide inclusions shown in Fig. 1 were observed in as-cast steel. Owing to the high cooling rate during solidification, these inclusions were considered to be the same as those in molten steel. The inclusions in as-cast steel were homogeneous and spherical; thus, it is assumed that liquid-yttrium-based oxide inclusions may be formed at steelmaking temperature. After heat treatment at temperatures of 1273 to 1573 K, a new gray phase with high yttrium content precipitated on the inclusions, as shown in Fig. 3. Most of the oxide inclusions changed from homogeneous to heterogeneous, even though some homogeneous inclusions were still observed in samples heated at 1273 and 1573 K. The morphology of inclusions also changed from spherical to irregular when the heating temperature was increased to 1473 and 1573 K (Figs. 3(d)–3(f)). Moreover, as illustrated in Fig. 9(b), the area fraction of inclusions in steels significantly increased with the increase in heating temperature. All of these results indicated that interfacial reaction between inclusions and steel matrix may have occurred and may be strengthened at high heating temperatures. Owing to the interfacial reaction, a product layer could form on the surface of inclusions at the initial isothermal holding and could spread to the inside of inclusions during heating. This could lead to the increase in area fraction of inclusions in steel.
On the basis of these experimental results, the evolution mechanism of yttrium-based oxide inclusions during isothermal heating at the temperatures of 1273 to 1573 K was considered to involve (i) the internal transformation of the oxide inclusions and (ii) the interfacial reaction between inclusions and solid stainless steel.
Considerable research on the phase evaluation, phase separation, and crystallization behavior of the Al2O3–Y2O3–SiO2 glass system during heat treatment from room temperature to 1623 K has been conducted [31–37]. Phase separation of the Al2O3–Y2O3–SiO2 glass had been observed during heating and was considered to be the early stage of crystallization [31–34]. In the present study, the Y/Al molar ratio of inclusions in as-cast steel was approximately 0.58, which nearly corresponded to that of the Al1.25Y0.75O3–SiO2 glass system. Related studies showed that 3Al2O3·2SiO2 (mullite) and Y2O3·2SiO2 phases precipitated from the Al1.25Y0.75O3–SiO2 system during long heat treatment periods because of crystallization, the starting temperature of crystallization was determined to be in the range of 1263 to 1323 K, and the maximum crystallization occurred between 1323 and 1523 K [31,33]. These conclusions are consistent with the results of the current work. As shown in Fig. 8, the most significant transformation of yttrium-based oxide inclusions into the Y-rich phase (gray phase, close to the Y2O3–SiO2 phase) and Al-rich phase (dark phase, close to the Al2O3–SiO2 phase) was observed during heating at 1373 K. Some unchanged oxide inclusions in samples heated at 1273 and 1573 K shown in Fig. 3 also indicated that the transformation of inclusions was restricted at low or high heating temperatures.
The results confirmed that MnO–SiO2-type inclusions in solid stainless steel could react with the steel matrix during heat treatment, resulting in the transformation of inclusions into MnO–Cr2O3-type particles [21–24]. Thus, the contribution of the interfacial reaction between homogeneous spherical Al–Y–Si(–Mn–Cr) oxide inclusions and steel matrix to the evolution of inclusions had also been considered. As shown in Fig. 8(b), the SiO2 content of the dark phase in inclusions obviously decreased after heating at temperatures of 1373 to 1573 K, whereas the MnO and Cr2O3 contents of the dark phase in inclusions increased. The reaction shown in Eq. (1) is expected to occur during heating [24].
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2[Cr]+2MnO⋅SiO2→MnO⋅Cr2O3+[Mn]+[Si],lgK=0.247−10269/T |
(1) |
where K means thermodynamic equilibrium constant of the reaction, T is reaction temperature (in Kelvin).
The thermodynamic affinity of yttrium for oxygen is stronger than that for alumina [38–39]. With the decrease in temperature from 1873 K to the heating temperatures of 1273 to 1573 K, the solubility of yttrium in the steel matrix would decrease. Thus, the excess yttrium in solid stainless steel would possibly diffuse to the surface of inclusions and react with the Al2O3 component in inclusions during heating, promoting the formation of the Y-rich phase. The possible reaction is shown in Eq. (2). Owing to the lack of thermodynamic data on this reaction at temperatures of 1273 to 1573 K, the related thermodynamic data on liquid steel is assumed to be applicable at the heating temperatures used in this study, as shown in Eq. (3) [40–41].
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2Y(inFCCiron)+Al2O3(ininclusion)=Y2O3(ininclusion)+2Al(inFCCiron) |
(2) |
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2[Y]+Al2O3(s)=Y2O3(s)+2[Al],ΔG⊖=−565768+268T |
(3) |
The standard states of Y and Al refer to those at a concentration of 1wt% in liquid Fe. The Gibbs energy (G) changes of this reaction at different heating temperatures (1273 to 1573 K) were calculated on the basis of the following assumptions: (1) the activity coefficient of Y and Al in steel reached unity because of their low concentrations in steel and (2) Al2O3 and Y2O3 were considered to be pure substances. The calculated results at 1273, 1373, 1473, and 1573 K were −231977, −205756, −179535, and −153314 J/mol, respectively. On the basis of the laws of thermodynamics, this reaction can occur during heating. However, the diffusion of alloy elements in solid stainless steel will be restricted at low heating temperatures, which may result in the inhibition of the interfacial reaction between inclusions and steel matrix. As shown in Fig. 3, the spherical shape of the oxide inclusions was retained after heating at 1273 and 1373 K, whereas irregular inclusions were observed after heating at 1473 and 1573 K. Moreover, the increase in area fraction of inclusions in steel became more obvious at high heating temperatures, as shown in Fig. 9(b). All of these findings indicate that the interfacial reaction between inclusions and steel matrix was suppressed at low heating temperatures. With the increase in temperature, the reaction was gradually induced.
Fig. 10 summarizes the proposed evolution mechanism of inclusions. At heating temperatures less than 1473 K (Zone I), internal transformation of yttrium-based oxide inclusions was considered to be the main factor because of the limitation of the diffusion of alloy elements (Y, Al, Mn, Cr, and Si) in solid stainless steel. During heating, Al3+ and O2− in inclusions diffused to the surface of the inclusion because of the crystallization of glassy oxide, resulting in the formation of a Y-rich phase on the edge of inclusions at 1273 K. With the increase in temperature to 1373 K, the Y-rich phase spread to the interior of the inclusion, and the Al-rich phase formed around the inclusion. Therefore, O, Al, Y, and Si concentration gradients existing within the gray phase in inclusions were observed, as shown in Fig. 6. When the heating temperature was continuously increased, the diffusion of alloy elements in steel became relatively easy. As shown in Zone II of Fig. 10, the elements [Y] and [Cr] diffused to the surface of the inclusion and induced the interfacial reaction, leading to the change in morphology of the inclusion from spherical to irregular and the increase in Cr2O3 content of the inclusion. Thus, the evolution mechanism of inclusions at high temperatures (1473 to 1573 K) was considered to be the combined effect of the internal transformation of inclusions and interfacial reaction between inclusions and steel matrix.
However, when the heating temperature is high, such as at 1573 K, the crystallization of inclusions would be suppressed to some extent [31,33], causing only a few inclusions to transform into heterogeneous inclusions with Y-rich and Al-rich parts. However, owing to the extensive interfacial reaction, some homogeneous oxide inclusions with high Cr2O3 content were formed, as shown in Fig. 3(f).
The effect of heating temperatures varying from 1273 to 1573 K on the evolution of yttrium-based oxide inclusions in solid stainless steel in terms of the morphology, composition, and size distribution during isothermal holding is investigated systematically. The following conclusions are drawn.
(1) Most of the homogeneous spherical Al–Y–Si(–Mn–Cr) oxide inclusions in as-cast steel transform into heterogeneous inclusions with Y-rich and Al-rich parts after heating at temperatures of 1273 to 1573 K.
(2) With the increase in heating temperature from 1273 to 1573 K, more large-sized oxide inclusions are observed in heated samples. The morphology of inclusions also change from spherical to irregular.
(3) The maximum transformation temperature of yttrium-based oxide inclusions during heat treatment is determined to be 1373 K.
(4) The evolution mechanism during heating at temperatures less than 1473 K is the internal transformation of inclusions due to the crystallization of glassy oxide. Meanwhile, the evolution mechanism during heating at high temperatures (1473 to 1573 K) is the combined effect of the (i) internal transformation of inclusions and (ii) interfacial reaction between inclusions and steel matrix.
This work was financially supported by the National Natural Science Foundation of China (Nos. 51574190 and 51734003), the Fundamental Research Funds for the Central Universities of China (No. FRF-TP-18-009C1), and the China Scholarship Council (No. 201806460049). The authors would also like to thank Prof. Simon N. Lekakh at Missouri University of Science and Technology for his guidance on this work.
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| 4. | Ji Chen, Hangyu Zhu, Lanqing Wang, et al. Effect of Yttrium Addition on Nonmetallic Inclusions in FeCrAl Alloys. steel research international, 2023, 94(12) DOI:10.1002/srin.202300212 |
| 5. | Yi Wang, Chang-rong Li, Lin-zhu Wang, et al. Effect of yttrium treatment on alumina inclusions in high carbon steel. Journal of Iron and Steel Research International, 2022, 29(4): 655. DOI:10.1007/s42243-021-00633-y |
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| Fe | Cr | Ni | Si | Mn | Total Al | Y | Total O |
| Bal. | 18 | 8 | 0.38 | 1.55 | 0.006 | 0.0085 | 0.011 |
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