Mechanism on Modification of MnO-SiO2-Type Oxide by Interfacial Solid-State Reaction During Heat Treatment

doi:10.11900/0412.1961.2016.00120

Acta Metall Sin

2017, Vol. 53

Issue (1): 10-18 DOI: 10.11900/0412.1961.2016.00120

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Mechanism on Modification of MnO-SiO₂-Type Oxide by Interfacial Solid-State Reaction During Heat Treatment

Chengsong LIU(

),Fei YE

The State Key Laboratory of Refractories and Metallurgy, Wuhan University of Science and Technology, Wuhan 430081, China

Cite this article:

Chengsong LIU,Fei YE. Mechanism on Modification of MnO-SiO₂-Type Oxide by Interfacial Solid-State Reaction During Heat Treatment. Acta Metall Sin, 2017, 53(1): 10-18.

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Abstract

In order to control physicochemical characteristics of inclusions in steel through appropriate heat treatment process, solid-state interface reaction between solid alloy deoxidized by Mn and Si and MnO-SiO₂-FeO oxide during heat treatment was studied. Using confocal scanning laser microscope (CSLM) and high temperature induction furnace, the reaction between the Fe-Mn-Si alloy and MnO-SiO₂-FeO oxide during heat treatment at 1473 K and its influence on the compositions and phases in the alloy and oxide were investigated by diffusion couple method. A suitable method for pre-melting oxide and producing diffusion couple of Fe-Mn-Si alloy and MnO-SiO₂-FeO oxide was proposed to obtain good contact between them. After that, the diffusion couple sample with Ti foil for reducing oxygen partial pressure and bulk alloy containing the same compositions was sealed in a quartz tube for carrying out subsequent heat treatment experiment. In addition, equilibrium compositions and phases of the oxide and alloy during solidification and the solid-state reaction mechanism between them were analyzed and discussed. Quantitative analysis of each element in alloy and oxide was calibrated by standard sample before analysis. Results showed that solid-state interface reaction and element diffusion between the Fe-Mn-Si alloy and MnO-SiO₂-FeO oxide were observed which indicated that the alloy and oxide in the diffusion couple was not equilibrated at 1473 K, even though the liquid phases of them were equilibrated at 1873 K. The activity of FeO in MnO-SiO₂-FeO oxide decreased with the decrease of temperature and excess oxygen diffused from oxide to alloy. Mn and Si contents in the alloy were consumed by the chemical reaction and some MnO-SiO₂ particles in the alloy near the interface generated. As the heat treatment time increased from 10 h to 50 h, the widths of particle precipitation zone (PPZ) and manganese depleted zone (MDZ) increased from 79 and 120 μm to 138 and 120 μm, respectively. During the heat treatment, the width of MDZ was always greater than that of PPZ. Moreover, due to the separation of the FeO, pure Fe particles formed in the oxide. The MnO and FeO contents in the oxide increased and decreased respectively with the increase of the heat treatment time.

Key words: oxide diffusion couple interfacial solid-state reaction heat treatment

Received: 06 April 2016

Fund: Supported by National Natural Science Foundation of China (No.51604201)

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https://www.ams.org.cn/EN/10.11900/0412.1961.2016.00120 OR https://www.ams.org.cn/EN/Y2017/V53/I1/10

Fig.1 Experimental set-up for pre-melting oxide in confocal scanning laser microscope (CSLM)

Fig.2 Schematic of the diffusion couple specimen sealed in a quartz tube

Fig.3 Temperature curve of the heat treatment for the diffusion couple specimen

Table 1 Chemical composition analyses of positions in Fig.4a

(mass fraction / %)

Fig.4 EPMA images of the interface between the alloy and oxide after the oxide pre-melting experiment (a), and after heat treatment at 1473 K for 10 h (b) and 50 h (c)

Table 2 Chemical composition analyses of positions in Fig.4b (mass fraction / %)

Table 3 Chemical composition analyses of positions in Fig.4c (mass fraction / %)

Fig.5 Changes of Mn (a) and Si (b) contents in the diffusion couple alloy after the oxide pre-melting experiment (specimen H-0), and after heat treatment at 1473 K for 10 h (specimen H-10) and 50 h (specimen H-50)

Fig.6 Width of particle precipitation zone (PPZ) and manganese depleted zone (MDZ) of the diffusion couple after the oxide pre-melting experiment, and after heat treatment at 1473 K for 10 and 50 h

Fig.7 Composition (a) and size distribution (b) of particles in the diffusion couple alloy near the interface after the oxide pre-melting experiment, and after heat treatment at 1473 K for 10 and 50 h

Fig.8 Changes in composition and phase in Fe-Mn-Si alloy (a) and MnO-SiO₂-FeO oxide (b) during solidification

Fig.9 Changes of activities of oxygen and FeO (a_O and a_FeO) with temperature in equilibrium calculation

Fig.10 Schematic for the mechanism of solid-state interface reaction between the alloy and inclusion

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