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ISIJ International
Vol. 51 (2011), No. 12

ISIJ International Vol. 51 (2011), No. 12

Preface to the Special Issue on “Fundamentals and Applications of Non-metallic Inclusions in Solid Steel”

Shin-ya Kitamura

pp. 1943-1943

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Preface to the Special Issue on “Fundamentals and Applications of Non-metallic Inclusions in Solid Steel”

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DOI:10.2355/isijinternational.51.1943
Recommended Articles: Behavior of Non-metallic Inclusions in Steel during Hot Deformation and the Effects of Deformed Inclusions on Local Ductility [ View more ]
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1. Behavior of Non-metallic Inclusions in Steel during Hot Deformation and the Effects of Deformed Inclusions on Local Ductility ISIJ International Vol.51(2011), No.12
2. Equilibrium Relationships between Oxide Compounds in MgO–Ti₂O₃–Al₂O₃ with Iron at 1873 K and Variations in Stable Oxides with Temperature ISIJ International Vol.51(2011), No.12
3. Thermodynamics of Si and Ti in Solid Fe at 1273 K ISIJ International Vol.51(2011), No.12
Mechanism of Change in Chemical Composition of Oxide Inclusions in Fe–Cr Alloys Deoxidized with Mn and Si by Heat Treatment at 1473 K

Hiroyuki Shibata, Koichiro Kimura, Tomoko Tanaka, Shin-ya Kitamura

pp. 1944-1950

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Mechanism of Change in Chemical Composition of Oxide Inclusions in Fe–Cr Alloys Deoxidized with Mn and Si by Heat Treatment at 1473 K

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DOI:10.2355/isijinternational.51.1944

Abstract

The MnO–SiO₂-type inclusions changed into MnO–Cr₂O₃ type inclusions in an Fe–Cr alloy deoxidised by Mn and Si with a low Si concentration by heat treatment at 1473 K. At high Si content, the MnO–SiO₂-type inclusion remained stable even after heat treatment. The change in the chemical composition of the oxide inclusions by heat treatment depended on the concentrations of Si and Cr in the Fe–Cr alloys. The mechanism of the change in the chemical composition of the oxide inclusions was investigated by using two experimental methods. The solubility of Cr₂O₃ in MnO–SiO₂ was measured from 1473 to 1673 K. The solubility of Cr₂O₃ decreased with temperature. The other experiment was performed using a diffusion couple method between the Fe–Cr alloy and MnO–SiO₂ at 1473 K to investigate a reaction between them. The formation of MnO–Cr₂O₃ was observed at the interface. It is found that both the decrease in solubility of Cr₂O₃ and diffusion of Mn, Cr, and Si at the interface between the Fe–Cr alloy and oxide inclusions are important for controlling the change in the chemical composition of the oxide inclusions in the Fe–Cr alloy by heat treatment at 1473 K.
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2. Changing Behavior of Non-metallic Inclusions in Solid Iron Deoxidized by Al–Ti Addition during Heating at 1473 K ISIJ International Vol.51(2011), No.12
3. Effect of Li₂O Addition on Crystallization Behavior of CaO–Al₂O₃–MgO Based Inclusions ISIJ International Vol.51(2011), No.12
Changing Behavior of Non-metallic Inclusions in Solid Iron Deoxidized by Al–Ti Addition during Heating at 1473 K

Wonjin Choi, Hiroyuki Matsuura, Fumitaka Tsukihashi

pp. 1951-1956

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Changing Behavior of Non-metallic Inclusions in Solid Iron Deoxidized by Al–Ti Addition during Heating at 1473 K

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DOI:10.2355/isijinternational.51.1951

Abstract

Changing behavior of non-metallic inclusions in composition and size distribution at high temperature was investigated by preparing three kinds of Fe–Al–Ti steels, heating at 1473 K, and observing inclusions by SEM-EDS. In the case of the specimen in which thermodynamically stable inclusion at 1873 K is Al₂O₃, mostly pure Al₂O₃ inclusions were observed in an as cast sample, while many dual phase inclusions were observed after heating. Iron content in inclusions increased and many Al–Ti–Fe–O inclusions in narrow composition range were observed. In the case of the specimen in which stable inclusion at 1873 K is Ti₃O₅, TiO_x inclusions were observed in an as cast sample. Inclusion compositions changed to Fe–Ti–O by heating and inclusion size became smaller to 2 to 3 μm. In the case of the specimen which composition is located at the boundary area of Al₂O₃, Al₂TiO₅, and Ti₃O₅ stable regions at 1873 K, various inclusions from pure Al₂O₃ to TiO_x were observed in an as cast sample. By heating, three types of inclusions, namely, Al₂O₃, Al–Fe–O, and Al–Ti–Fe–O inclusions were observed and average inclusion size decreased. Although the stable phase of oxide equilibrated with Fe–Al–Ti–O system at 1473 K are not clarified, inclusions equilibrated with molten metal are no longer stable in solid state steel and thus inclusion composition and size change by reacting with solid steel.
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1. Atmosphere Controlled Hot Thermocouple Method and Crystallization Phenomenon of CaO–Al₂O₃ Eutectic Slag ISIJ International Vol.51(2011), No.12
2. Mechanism of Change in Chemical Composition of Oxide Inclusions in Fe–Cr Alloys Deoxidized with Mn and Si by Heat Treatment at 1473 K ISIJ International Vol.51(2011), No.12
3. Effect of Li₂O Addition on Crystallization Behavior of CaO–Al₂O₃–MgO Based Inclusions ISIJ International Vol.51(2011), No.12
Investigation of Compositional Change of Inclusions in Martensitic Stainless Steel during Heat Treatment by Newly Developed Analysis Method

Toru Taniguchi, Naoya Satoh, Yoichiro Saito, Kunichika Kubota, Atsushi Kumagai, Yasushi Tamura, Takahiro Miki

pp. 1957-1966

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Investigation of Compositional Change of Inclusions in Martensitic Stainless Steel during Heat Treatment by Newly Developed Analysis Method

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DOI:10.2355/isijinternational.51.1957

Abstract

The most important subject in the steelmaking process is the control of non-metallic inclusions. Non-metallic inclusions with a high melting point do not deform during a hot working process because they are relatively hard. Hence, the inclusion composition should be controlled in order to achieve a low melting point to prevent product defects. Therefore, an MnO–SiO₂-based inclusion is considered to be one of the preferred systems.
Moreover, the heat treatment of austenitic stainless steel has been reported to influence the composition of MnO–SiO₂-type inclusions; these inclusions change into MnO–Cr₂O₃-type, MnO–Nb₂O₅-type, and MnO–V₂O₃-type inclusions.
In this study, we investigated the influence of heat treatment on the composition of the inclusions in the martensitic stainless steel.
In general, a scanning electron microscope–energy dispersive x-ray spectrometer (SEM–EDS) is used for the quantitative analysis of inclusions; however, SEM–EDS cannot simultaneously analyze a large number of inclusions. Therefore, a new technique using the SEM–EDS along with the image analysis software “Particle Analysis” was used for the chemical analysis and the size measurement of a large number of inclusions (hereafter abbreviated as the PA method). The heat-treatment-induced compositional change of the inclusions in martensitic stainless steel was evaluated by using both the analysis methods.
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1. Application of Statistics of Extreme Values for Inclusions in Stainless Steel on Different Stages of Steel Making Process ISIJ International Vol.51(2011), No.12
2. Behavior of Non-metallic Inclusions in Steel during Hot Deformation and the Effects of Deformed Inclusions on Local Ductility ISIJ International Vol.51(2011), No.12
3. Effect of Heat Treatment Conditions on Shape Control of Large-sized Elongated MnS Inclusions in Resulfurized Free-cutting Steels ISIJ International Vol.51(2011), No.12
Atmosphere Controlled Hot Thermocouple Method and Crystallization Phenomenon of CaO–Al₂O₃ Eutectic Slag

Yoshiaki Kashiwaya, Yasuaki Kusada, Ryosuke O. Suzuki

pp. 1967-1973

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Atmosphere Controlled Hot Thermocouple Method and Crystallization Phenomenon of CaO–Al₂O₃ Eutectic Slag

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DOI:10.2355/isijinternational.51.1967

Abstract

A desulfurization slag is difficult to recycle, since there is a possibility to elute a sulfur containing solution. To promote the recycle of the desulfurization slags, it is important to know the physicochemical properties of the slag. In addition, desulfurization process could be modified, when the sulfur behavior in the slag was understood.
In this study, the effect of sulfur and oxygen partial pressure on the crystallization behavior was investigated using Hot Thermocouple Technique. Three different atmospheres were established in the electric furnace through the modification of experimental apparatus. One was an argon without deoxidation, the second was an argon with Ti plate (Ar+Ti) which was located in the electric furnace for deoxidation of argon gas, and the third was an argon with CaS pellet located on the Ti plate (Ar+Ti+CaS) in which the partial pressure of SO₂ increased with the decrease of the oxygen partial pressure.
The nose position of TTT diagram of CaO–Al₂O₃ eutectic composition under Ar atmosphere was 7 s at 1100°C, while the nose positions under Ar+Ti and Ar+Ti+CaS were 7 s at 1150°C. TTT diagrams under Ar+Ti and Ar+Ti+CaS, which are lower oxygen potential and higher SO₂ potential, showed the earlier crystallization behavior in the higher temperature region than the nose position. From the results of XRD analysis, the sulfur added to the slag existed in the monocalcium aluminate (CaO·Al₂O₃) primary crystal. When the content of CaS increased, a formation of CaO through oxidation increased and the tricalcium aluminate (3CaO·Al₂O₃) was formed as a primary crystal, in which the sulfur content was higher than the eutectic structure in the matrix.
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2. Mechanism of Change in Chemical Composition of Oxide Inclusions in Fe–Cr Alloys Deoxidized with Mn and Si by Heat Treatment at 1473 K ISIJ International Vol.51(2011), No.12
3. Effect of Li₂O Addition on Crystallization Behavior of CaO–Al₂O₃–MgO Based Inclusions ISIJ International Vol.51(2011), No.12
Effect of Sulfur on the TTT Diagram of CaO–Al₂O₃ Slag at Eutectic Composition

Yoshiaki Kashiwaya, Yasuaki Kusada, Ryosuke O. Suzuki

pp. 1974-1981

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Effect of Sulfur on the TTT Diagram of CaO–Al₂O₃ Slag at Eutectic Composition

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DOI:10.2355/isijinternational.51.1974

Abstract

It is important to know the behavior of inclusion in a CaO–Al₂O₃-(SiO₂ and/or MgO) system for controlling the properties of steel. The crystallization of inclusion has a large effect on the rolling process. However, there is little study of the effect of sulfur on the crystallization of inclusion. In the previous paper, the authors were investigated the sulfur behavior in the CaO–Al₂O₃ slag at the eutectic composition (CA_EU) under controlled atmosphere. In the present study, the effects of sulfur on the TTT diagrams were measured by the hot thermocouple method under controlled atmosphere. 1 mass%, 5 mass% and 10 mass% CaS were added to the eutectic composition of calcium aluminate (CA_EU).
The crystal region in TTT diagrams was expanded by the addition of CaS from 1 mass% to 10 mass% under Ar atmosphere. And the start of crystallization became faster with the increase of CaS addition. The crystal phases were monocalcium aluminate (CA) and tricalcium aluminate (C₃A) regardless to the CaS content. However, primary crystal was changed from the content of CaS. When 1 mass%CaS was added to CA_EU, the primary crystal was CA. On the other hand, the primary crystal was C₃A in the cases of 5 mass% and 10 mass%CaS.
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2. Effect of V, Nb and Ti Addition and Annealing Temperature on Microstructure and Tensile Properties of AISI 301L Stainless Steel ISIJ International Vol.51(2011), No.6
3. Effect of Acicular Ferrite on Cracking Sensibility in the Weld Metal of Q690+Q550 High Strength Steels ISIJ International Vol.51(2011), No.7
Effect of Li₂O Addition on Crystallization Behavior of CaO–Al₂O₃–MgO Based Inclusions

Tomoko Sugimura, Tetsushi Deura, Koichi Sakamoto, Sohei Sukenaga, Noritaka Saito, Kunihiko Nakashima

pp. 1982-1986

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Effect of Li₂O Addition on Crystallization Behavior of CaO–Al₂O₃–MgO Based Inclusions

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DOI:10.2355/isijinternational.51.1982

Abstract

The crystallization behavior of CaO–Al₂O₃–MgO oxide powder which is one of the major non-metallic inclusions in Al-killed steel was systematically examined in the present study. 33mass%CaO–62mass% Al₂O₃–5mass%MgO and 30mass%CaO–57mass% Al₂O₃–5mass%MgO–8mass%Li₂O glass powders were heat-treated at 1073–1673 K for 8–512 s under air.
CaO–Al₂O₃–MgO glass was found to be crystallized immediately after the heat treatments. Moreover, it was revealed that the addition of Li₂O accelerated the crystallization of the glass powders, and controlled aggregation of crystal particles. Additionally, the indentation hardness of crystallized glasses after 512 s heat-treatments was investigated by using a nano-indenter. The addition of Li₂O had the effect of lowering the hardness of samples, which indicates that Li₂O would improve the deformation behavior of aluminate based inclusions.
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3. Atmosphere Controlled Hot Thermocouple Method and Crystallization Phenomenon of CaO–Al₂O₃ Eutectic Slag ISIJ International Vol.51(2011), No.12
Behavior of Non-metallic Inclusions in Steel during Hot Deformation and the Effects of Deformed Inclusions on Local Ductility

Ken-ichi Yamamoto, Hideaki Yamamura, Yoshihiro Suwa

pp. 1987-1994

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Behavior of Non-metallic Inclusions in Steel during Hot Deformation and the Effects of Deformed Inclusions on Local Ductility

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DOI:10.2355/isijinternational.51.1987

Abstract

In order to clarify both the behavior of non-metallic inclusions during hot deformation and the effects of non-metallic inclusions on the local ductility of steel with aluminum deoxidized and containing lower sulfur content at about 0.002–0.01% were investigated. Both the commercial-quality 440 MPa-class plain carbon steel and super ultra-low carbon steel were studied. To investigate the distribution, morphology, and chemical composition, along with the change in such characteristics, during the hot deformation of non-metallic inclusions, thermo-mechanical treatment with a compression test was carried out. Moreover, the reduction of area with the tensile test species, which refers to the local ductility of steel, was examined, and the effect of the distribution, morphology, and chemical compositions of both the Al₂O₃ inclusions and the elongated MnS inclusions were studied.
Consequently, metal sulfur content of higher than 60 ppm and elongated MnS inclusions of over 10 regarding the aspect ratio were observed. In addition, the elongated MnS inclusions had a stronger influence on local ductility than the smaller Al₂O₃ inclusions, and drastic effects on the nucleation of voids. Thus, a fracture is most likely to be initiated by void formation at the interface of the elongated MnS inclusions and metal matrix notched by MnS, and thus would experience coalescence in accordance with a brittle fracture in the soft MnS inclusions. The local ductility in steel including elongated MnS inclusions is small because the fracturing and deformation of metal are most likely to be related to the elongated MnS inclusions.
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1. Investigation of Compositional Change of Inclusions in Martensitic Stainless Steel during Heat Treatment by Newly Developed Analysis Method ISIJ International Vol.51(2011), No.12
2. Preface to the Special Issue on “Fundamentals and Applications of Non-metallic Inclusions in Solid Steel” ISIJ International Vol.51(2011), No.12
3. Effect of Heat Treatment Conditions on Shape Control of Large-sized Elongated MnS Inclusions in Resulfurized Free-cutting Steels ISIJ International Vol.51(2011), No.12
Effect of Heat Treatment Conditions on Shape Control of Large-sized Elongated MnS Inclusions in Resulfurized Free-cutting Steels

Xiaojing Shao, Xinhua Wang, Min Jiang, Wanjun Wang, Fuxiang Huang

pp. 1995-2001

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Effect of Heat Treatment Conditions on Shape Control of Large-sized Elongated MnS Inclusions in Resulfurized Free-cutting Steels

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DOI:10.2355/isijinternational.51.1995

Abstract

Effect of heat treatment conditions on shape evolution of large-sized elongated MnS inclusions in resulfurized free-cutting rolled steel has been investigated using confocal scanning laser microscope and Si₂Mo resistance furnace. The results show that the heating rate, soaking temperature and soaking time impose significant effects upon shape profiles of elongated MnS. The split of slender MnS was oberved in continuous heating with heating rate in the range of 0.5–2 K/s. In addition, split degree of MnS indicated a negative relation with the rise of heating rate. As a result, separation of elongated MnS was not observed at the heating rate of 6 K/s. During soaking experiments, there was no remarkable shape change for MnS at temperature lower than 1073 K. While the elongated MnS splited up and spheroidized obviously at 1473 K. Correspondingly, number density of inclusions increased while mean length reduced as the soaking time increased from 1 h to 4 h at 1473 K. Significant shape change from slender to spindlelike or spherical was identified only when the soaking time exceeds 3 h or 4 h. Based on the Gibbs Thompson relation and the obtained experimental results, mechanism of shape evolution of MnS inclusions was discussed and morphology evolution of MnS was divided into three major steps: (1) first, the shrinkage occurred in the longitudinal direction at the beginning of heating process, (2) expansion and contraction in radial direction followed after the shrinkage which caused the split of slender MnS; (3) eventually, the spherical particles emerged from the split parts.
Recommended Articles: Effect of Sulfur on the TTT Diagram of CaO–Al₂O₃ Slag at Eutectic Composition [ View more ]
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1. Effect of Sulfur on the TTT Diagram of CaO–Al₂O₃ Slag at Eutectic Composition ISIJ International Vol.51(2011), No.12
2. Investigation of Compositional Change of Inclusions in Martensitic Stainless Steel during Heat Treatment by Newly Developed Analysis Method ISIJ International Vol.51(2011), No.12
3. Behavior of Non-metallic Inclusions in Steel during Hot Deformation and the Effects of Deformed Inclusions on Local Ductility ISIJ International Vol.51(2011), No.12
Thermodynamics of Si and Ti in Solid Fe at 1273 K

Youngjo Kang, Kazuki Morita

pp. 2002-2006

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Thermodynamics of Si and Ti in Solid Fe at 1273 K

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DOI:10.2355/isijinternational.51.2002

Abstract

Equilibrium experiments were carried out with solid Fe and liquid Ag to investigate the interactions between Si and Ti in solid Fe. The thermodynamic properties of Si in γ-Fe and α-Fe phases were studied by determining the distribution equilibrium of Si in the Fe and the Ag phases. Using the activity coefficient and the self-interaction parameter of Si in solid Fe, the interaction parameter of Si and Ti in both the solid Fe phases— γ-Fe and α-Fe—was determined as follows:
ε_Si^Ti = 460 ± 78 in γ-Fe, ε_Si^Ti = 350 ± 7 in α-Fe
The analysis results for Si and Ti in the solid Fe phase showed reasonable agreement with previous research in α-Fe region. Furthermore, the influence of the interaction between Si and Ti in the solid Fe phases on the formation of secondary inclusions such as Ti-based inclusions was discussed. It was concluded that, during solidification, the interactions among solutes such as Si and Ti should be properly considered because the formation of not only the secondary inclusions but also ferrites may depend on the thermodynamic properties of the solutes.
Recommended Articles: Changing Behavior of Non-metallic Inclusions in Solid Iron Deoxidized by Al–Ti Addition during Heating at 1473 K [ View more ]
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1. Changing Behavior of Non-metallic Inclusions in Solid Iron Deoxidized by Al–Ti Addition during Heating at 1473 K ISIJ International Vol.51(2011), No.12
2. Mechanism of Change in Chemical Composition of Oxide Inclusions in Fe–Cr Alloys Deoxidized with Mn and Si by Heat Treatment at 1473 K ISIJ International Vol.51(2011), No.12
3. Atmosphere Controlled Hot Thermocouple Method and Crystallization Phenomenon of CaO–Al₂O₃ Eutectic Slag ISIJ International Vol.51(2011), No.12
Phase Equilibrium between CaO·Al₂O₃ Saturated Molten CaO–Al₂O₃–MnO and (Ca, Mn)S Solid Solution

Hiroshi Fukaya, Takahiro Miki

pp. 2007-2011

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Phase Equilibrium between CaO·Al₂O₃ Saturated Molten CaO–Al₂O₃–MnO and (Ca, Mn)S Solid Solution

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DOI:10.2355/isijinternational.51.2007

Abstract

Refinement of austenite grains by generating intra granular ferrite (IGF) in austenite grains is one of the most effective methods for improving the toughness of the heat-affected zone (HAZ). It is known that MnS precipitated on fine oxides enhance formation of IGF in austenite grains. Flux composed of CaO–Al₂O₃ is often used in secondary refining and Ca–Mn–Al complex oxide may form, and it is important to clarify the mechanism of MnS precipitation on oxide inclusions. Therefore, molten CaO–MnO–Al₂O₃ oxide was equilibrated with (Ca, Mn)S solid solution in Al₂O₃ crucible in an electric resistance furnace at 1648, 1698 and 1748 K in the present work. Phase relation between CaO·Al₂O₃ saturated molten CaO–MnO–Al₂O₃ oxide and (Ca, Mn)S solid solution was clarified.
Recommended Articles: Changing Behavior of Non-metallic Inclusions in Solid Iron Deoxidized by Al–Ti Addition during Heating at 1473 K [ View more ]
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1. Changing Behavior of Non-metallic Inclusions in Solid Iron Deoxidized by Al–Ti Addition during Heating at 1473 K ISIJ International Vol.51(2011), No.12
2. Mechanism of Change in Chemical Composition of Oxide Inclusions in Fe–Cr Alloys Deoxidized with Mn and Si by Heat Treatment at 1473 K ISIJ International Vol.51(2011), No.12
3. Atmosphere Controlled Hot Thermocouple Method and Crystallization Phenomenon of CaO–Al₂O₃ Eutectic Slag ISIJ International Vol.51(2011), No.12
Equilibrium Relationships between Oxide Compounds in MgO–Ti₂O₃–Al₂O₃ with Iron at 1873 K and Variations in Stable Oxides with Temperature

Hideki Ono, Toshio Ibuta

pp. 2012-2018

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Equilibrium Relationships between Oxide Compounds in MgO–Ti₂O₃–Al₂O₃ with Iron at 1873 K and Variations in Stable Oxides with Temperature

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DOI:10.2355/isijinternational.51.2012

Abstract

It is important to determine the equilibrium relationships between the oxide compounds in MgO–Ti₂O₃–Al₂O₃ and iron to avoid Al₂O₃ or MgO·Al₂O₃ formation and for inclusion control. In this study, the equilibrium relationships between the oxide compounds in MgO–Ti₂O₃–Al₂O₃ and molten iron are investigated at 1873 K. The phase-stability diagrams, which show the equilibrium relationships between the oxide compounds in MgO–Ti₂O₃–Al₂O₃ and molten iron, are described. It is also important to know the oxides that newly form after solidification. Accordingly, the temperature-dependences of the stable compounds that newly form after solidification were investigated using the thermodynamic calculation software FactSage 6.1. Although the compounds formed after solidification are not necessarily the same as the equilibrium oxide compounds at 1873 K, the correlation between them can be confirmed. In particular, under the unstable condition of MgAl₂O₄ at 1873 K, it is found that the formation of MgAl₂O₄ could also be suppressed after solidification.
Recommended Articles: Changing Behavior of Non-metallic Inclusions in Solid Iron Deoxidized by Al–Ti Addition during Heating at 1473 K [ View more ]
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1. Changing Behavior of Non-metallic Inclusions in Solid Iron Deoxidized by Al–Ti Addition during Heating at 1473 K ISIJ International Vol.51(2011), No.12
2. Mechanism of Change in Chemical Composition of Oxide Inclusions in Fe–Cr Alloys Deoxidized with Mn and Si by Heat Treatment at 1473 K ISIJ International Vol.51(2011), No.12
3. Atmosphere Controlled Hot Thermocouple Method and Crystallization Phenomenon of CaO–Al₂O₃ Eutectic Slag ISIJ International Vol.51(2011), No.12
Micro-structure Refinement in Low Carbon High Manganese Steels through Ti-Deoxidation, Characterization and Effect of Secondary Deoxidation Particles

Naoki Kikuchi, Seiji Nabeshima, Takako Yamashita, Yasuo Kishimoto, Seetharaman Sridhar, Tetsuya Nagasaka

pp. 2019-2028

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Micro-structure Refinement in Low Carbon High Manganese Steels through Ti-Deoxidation, Characterization and Effect of Secondary Deoxidation Particles

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DOI:10.2355/isijinternational.51.2019

Abstract

This paper investigates the effect of de-oxidation inclusions on micro-structure in low carbon (0.07 mass%), high Mn (0.9 mass%) steel. De-oxidation tests were carried out by adding either aluminum (0.05 mass%) or titanium (0.05, 0.03 or 0.015 mass%) to an iron melt in a 400 g-scale vacuum furnace. A Confocal Scanning Laser Microscope (CSLM) was used to evaluate the effect of cooling rate by re-melting and quenching during solidification. Fine secondary de-oxidation particles were obtained in the Ti-killed samples, and the particle density increased with increasing oxygen content, and their size decreased with increasing the cooling rate during solidification.
The secondary Ti de-oxidation particles were found to have an effect on microstructure evolution, such as solidifying microstructure, austenite grain growth and austenite decomposition. The de-oxidation particles were examined through FE-TEM and were identified to be TiO, MnTiO₃ and Mn₂TiO₄, in low oxygen ([O]=7 ppm) and high oxygen ([O]=56, 81 ppm) Ti-killed steels respectively, which were qualitatively same as those predicted by thermodynamic calculations. Stabilities of TiO, MnTiO₃ and Mn₂TiO₄ are influenced by Mn presence. Composition change and decomposition of oxide were estimated through thermodynamic calculations. The effect of the particles on ferrite formation was evaluated through thermo-mechanical treatments. TiO was the most effective for promoting ferrite formation through heterogeneous nucleation. The particles contributed to ferrite formation in the following order, TiO>TiN>MnS> MnTiO₃>Ti₂O₃.
It was found that the secondary Ti de-oxidation particles work are engulfed by the advancing solid phase during solidification based on analysis with PET (Pushing Engulfment Transition) velocity, particle sizes and solidification rates. The particles at dendrite tips and inter-dendritic regions are likely restraining the molten steel flow resulting in a finer solidification microstructure.
Recommended Articles: Micro-structure Refinement in Low Carbon High Manganese Steels through Ti-deoxidation—Inclusion Precipitation and Solidification Structure [ View more ]
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1. Micro-structure Refinement in Low Carbon High Manganese Steels through Ti-deoxidation—Inclusion Precipitation and Solidification Structure ISIJ International Vol.48(2008), No.7
2. Characteristic Transformation of Manganese-containing Inclusions during Al-killed Process in Ultra-low Carbon Interstitial-free Steel ISIJ International Vol.58(2018), No.5
3. Changing Behavior of Non-metallic Inclusions in Solid Iron Deoxidized by Al–Ti Addition during Heating at 1473 K ISIJ International Vol.51(2011), No.12
Effect of Ti and Al Addition on Solidification Structure of Ni–Fe–Mo–Cu Alloys

Katsunari Oikawa, Hidekazu Todoroki, Masayuki Kubota, Kouichi Anzai

pp. 2029-2035

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Effect of Ti and Al Addition on Solidification Structure of Ni–Fe–Mo–Cu Alloys

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DOI:10.2355/isijinternational.51.2029

Abstract

The effect of the addition of Ti and Al on the solidification structure of Ni–4%Mo–5%Cu–13%Fe (mass%) alloys was investigated. It was found that the addition of an optimal amount of both Ti and Al affects on the formation of equiaxed fine grains. Oxide films formed on the molten alloy surface (scum) were examined using a transmission electron microscope equipped with energy dispersive spectrometers. The scum was analyzed and found to contain two separated phases of TiO with the monoclinic structure and Al₂O₃ with the corundum structure. The TiO might be the NaCl structure at the melting point of the matrix phase.
According to the lattice disregistry between the fcc Ni and oxides TiO with the NaCl structure has lower disregistry than Al₂O₃ with the corundum structure. These facts suggest that TiO precipitated with Al₂O₃ in Ni melt can form heterogeneous nucleation sites for the fcc Ni phase. The distribution conditions of TiO may be different between the Ti-added alloys and those with the addition of both Al and Ti. It is considered that the addition of both Al and Ti causes fine dispersion of TiO and promotes nucleation of the primary fcc Ni phase.
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1. Changing Behavior of Non-metallic Inclusions in Solid Iron Deoxidized by Al–Ti Addition during Heating at 1473 K ISIJ International Vol.51(2011), No.12
2. Mechanism of Change in Chemical Composition of Oxide Inclusions in Fe–Cr Alloys Deoxidized with Mn and Si by Heat Treatment at 1473 K ISIJ International Vol.51(2011), No.12
3. Atmosphere Controlled Hot Thermocouple Method and Crystallization Phenomenon of CaO–Al₂O₃ Eutectic Slag ISIJ International Vol.51(2011), No.12
Ferrite Formation Behaviors from B1 Compounds in Steels

Changjoon Lee, Shoichi Nambu, Junya Inoue, Toshihiko Koseki

pp. 2036-2041

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Ferrite Formation Behaviors from B1 Compounds in Steels

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DOI:10.2355/isijinternational.51.2036

Abstract

The effect of chemical composition of B1 compounds on the formation of intragranular ferrite during isothermal austenite-to-ferrite transformation was investigated by embedding single crystalline grains of chemically pure B1 compounds in low-alloy steel. Two kinds of B1 compounds having similar misfit against ferrite, TiO and TiN, were adopted in this study. Isothermal transformation experiments were carried out both above and below the bainitic transformation temperature. The orientation relationships between compound and ferrite and between ferrite and prior austenite were characterized by scanning electron microscope equipped with electron backscatter diffraction analyzer.
It was found that the Baker-Nutting (B-N) orientation relationship played a dominant role in ferrite formation from B1 compounds at higher transformation temperature, but some low-index orientation relationships other than the Baker-Nutting orientation relationship were also observed as the transformation temperature decreased, which led to an increase in ferrite formation having the Kurdjumov-Sachs (K-S) orientation relationship with prior austenite. Ferrites from TiO had larger misorientation angles from the exact B-N orientation relationship and thus tended to have the K-S orientation relationship with prior austenite at lower transformation temperatures.
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1. Changing Behavior of Non-metallic Inclusions in Solid Iron Deoxidized by Al–Ti Addition during Heating at 1473 K ISIJ International Vol.51(2011), No.12
2. Mechanism of Change in Chemical Composition of Oxide Inclusions in Fe–Cr Alloys Deoxidized with Mn and Si by Heat Treatment at 1473 K ISIJ International Vol.51(2011), No.12
3. Atmosphere Controlled Hot Thermocouple Method and Crystallization Phenomenon of CaO–Al₂O₃ Eutectic Slag ISIJ International Vol.51(2011), No.12
Application of Laser Ablation ICP Mass Spectrometry for Analysis of Oxide Particles on Cross Section of Alloys and Steels

Andrey Vladimirovich Karasev, Hideaki Suito, Ryo Inoue

pp. 2042-2049

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Application of Laser Ablation ICP Mass Spectrometry for Analysis of Oxide Particles on Cross Section of Alloys and Steels

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DOI:10.2355/isijinternational.51.2042

Abstract

Some aspects for the application of Laser Ablation-Inductively Coupled Plasma Mass Spectrometry (LA-ICP-MS) are considered and discussed from the viewpoint of the rapid analysis of oxide inclusions in metal samples. The inclusion characteristics in Fe–10% Ni alloy samples such as number, size and particle size distribution obtained by LA-ICP-MS method are compared with those from three-dimensional observation of particles on a film filter after electrolytic extraction. Though some limits had to be considered regarding to the content of soluble elements, the number and dispersion of analyzed inclusions in metal matrix, it was found that the LA-ICP-MS technique can be successfully applied for the rapid analysis of oxide inclusions containing Al₂O₃, MgO and others.
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1. Changing Behavior of Non-metallic Inclusions in Solid Iron Deoxidized by Al–Ti Addition during Heating at 1473 K ISIJ International Vol.51(2011), No.12
2. Mechanism of Change in Chemical Composition of Oxide Inclusions in Fe–Cr Alloys Deoxidized with Mn and Si by Heat Treatment at 1473 K ISIJ International Vol.51(2011), No.12
3. Atmosphere Controlled Hot Thermocouple Method and Crystallization Phenomenon of CaO–Al₂O₃ Eutectic Slag ISIJ International Vol.51(2011), No.12
Extraction of Nonmetallic Inclusion Particles Containing MgO from Steel

Ryo Inoue, Shigeru Ueda, Tatsuro Ariyama, Hideaki Suito

pp. 2050-2055

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Extraction of Nonmetallic Inclusion Particles Containing MgO from Steel

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DOI:10.2355/isijinternational.51.2050

Abstract

Extraction of inclusion particles from a metal matrix allows for accurate three-dimensional estimation of their morphology, size, and composition. In this study, the stability of MgO and MgAl₂O₄ particles was examined using acid, halogen-methanol, and nonaqueous electrolytes. These particles hardly dissolved in a 2% TEA-Ba (2 v/v% triethanolamine-1 w/v% tetramethylammoniumchloride-methanol containing 0.05–0.20 w/v% Ba) electrolyte. The potentiostatic extraction method using nonaqueous electrolytes with various Ba and H₂O contents was examined for the extraction of MgO inclusion particles from metals. The O content of the extracted MgO and MgAl₂O₄ inclusion particles agreed approximately with the analyzed total O content of the metal. The Mg contents of the extracted inclusion particles were in agreement with those calculated using the results of two-dimensional measurements. Finally, it was concluded that 2% TEA-Ba was the most suitable for the electrolytic extraction of MgO and MgAl₂O₄ inclusion particles from steel.
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1. Apparent Morphologies of Coarse Plate Martensite ISIJ International Vol.44(2004), No.4
2. Characteristics of Iron Entrainment into Slag Due to Rising Gas Bubbles ISIJ International Vol.43(2003), No.11
3. Simulation of the Estimation of the Maximum Inclusion Size from 2-Dimensional Observation Data on the Basis of the Extreme Value of Statistics ISIJ International Vol.49(2009), No.7
Application of Statistics of Extreme Values for Inclusions in Stainless Steel on Different Stages of Steel Making Process

Yuichi Kanbe, Andrey Karasev, Hidekazu Todoroki, Pär Göran Jönsson

pp. 2056-2063

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Application of Statistics of Extreme Values for Inclusions in Stainless Steel on Different Stages of Steel Making Process

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DOI:10.2355/isijinternational.51.2056

Abstract

A statistics of extreme values was applied to determine the largest inclusion sizes in the Type 304 stainless steel. The samples taken from a tundish, slab and hot rolled steel in one heat were examined by using a two dimensional observation of inclusions on a metal cross section. It was found that the molten steel sample contained two different types of inclusions, which were deoxidation products (SiO₂–CaO–MgO–Al₂O₃) and reoxidation products (SiO₂–MnO–Cr₂O₃). As a result, the extreme value distribution (EVD) for different types of inclusions in the melt has two different slopes. Meanwhile, the inclusions in the slab sample provided a good linearity in one EVD. Moreover, the correlation coefficients of the regression lines for both the slab and rolled steel samples increased significantly with an increased number of measurements from 40 to 80 unit areas. It was found also that the EVD data for fractured inclusions on a parallel cross section of rolled steel agreed satisfactorily well with that for the initial spherical inclusions in the slab sample. Based on the geometrical considerations of inclusion deformation and fracture during hot-rolling, the maximum length of fractured inclusions in rolled steel can be estimated reasonably well from the EVD for initial undeformed inclusions in the slab sample.
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1. Formation Mechanism of Non-Metallic Inclusions in Different Stainless Steel Grades ISIJ International Vol.43(2003), No.8
2. Control of Formation of Spinel Inclusion in Type 304 Stainless Steel by Slag Composition Tetsu-to-Hagané Vol.93(2007), No.7
3. Refining Technology for High Purity Stainless Steels and Some Properties of Products Tetsu-to-Hagané Vol.70(1984), No.11
Effect of Observed Number of Inclusions on the Diameter Distribution at Two-Dimensional Inspection

Atsushi Okayama, Takayuki Nishi

pp. 2064-2068

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Effect of Observed Number of Inclusions on the Diameter Distribution at Two-Dimensional Inspection

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DOI:10.2355/isijinternational.51.2064

Abstract

The effects of observed number of inclusions on the diameter distribution at two-dimensional inspection were evaluated in this work. Microscopic observations were reproduced by numerical calculations. Numerically calculated diameters of circles at cross-sectional planes were aggregated as size and density histograms and those were compared with theoretically calculated histograms. Deviations between the calculated and true density in each class were evaluated quantitatively with the error evaluation index.
The reliability of two-dimensional particle size and density histogram was affected by the observed number of particles rather than the observed number of fields and independent of the input three-dimensional particle distribution. Misunderstandings in reading the histograms could be prevented by setting small number of classes when the observed number of particles is small. It is better to decide the goal of reliability level before inspection to optimize the observation time and cost.
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1. Changing Behavior of Non-metallic Inclusions in Solid Iron Deoxidized by Al–Ti Addition during Heating at 1473 K ISIJ International Vol.51(2011), No.12
2. Mechanism of Change in Chemical Composition of Oxide Inclusions in Fe–Cr Alloys Deoxidized with Mn and Si by Heat Treatment at 1473 K ISIJ International Vol.51(2011), No.12
3. Atmosphere Controlled Hot Thermocouple Method and Crystallization Phenomenon of CaO–Al₂O₃ Eutectic Slag ISIJ International Vol.51(2011), No.12
Magnesium Non-metallic Inclusions in Non-oriented Electrical Steel Sheets

Darja Steiner Petrovič, Boštjan Arh, Franc Tehovnik, Miran Pirnat

pp. 2069-2075

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Magnesium Non-metallic Inclusions in Non-oriented Electrical Steel Sheets

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DOI:10.2355/isijinternational.51.2069

Abstract

During routine metallographic investigations of some fully processed, non-oriented, electrical steel sheets, the typical MnS inclusions were not observed in the microstructures. In the MS-type sulphides, the manganese was substituted by magnesium. A systematic ex-situ characterisation of the non-metallic, magnesium-containing inclusions was carried out and the origin of the inclusions was proposed. The inclusions' chemistry and morphology were investigated by light microscopy and field-emission scanning electron microscopy. The non-metallic, magnesium-containing inclusions were classified as complex sulphides, oxides and spinels. Magnesium was also detected as being co-precipitated with other non-metallic inclusions, like nitrides. The form of the co-precipitated magnesium inclusions was predetermined by the shape of the thermodynamically most stable inclusions.
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