锆脱氧钢中非金属夹杂物的表征及对比分析

doi:10.3964/j.issn.1000-0593(2023)09-2916-06

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Abstract The comprehensive and accurate characterization of the characteristics of non-metallic inclusions in steel is conducive to the discovery and recognition of new inclusions and is also the prerequisite for the regulation of non-metallic inclusions and the improvement of steel quality. This paper uses scanning electron microscopy with energy spectrum (SEM-EDS), Raman spectrum, high-resolution transmission electron microscope(TEM) and micro-region X-ray diffraction (μXRD), combined with the inclusion of electrolytic extraction technology and image analysis technology, the characterization of zirconium deoxidization non-metallic inclusions in steel shape, size, quantity, distribution, composition, crystal structure, characteristic parameters such as comparative analysis the advantages and disadvantages of four kinds of methods for characterizing the inclusions. The results show that the inclusion in zirconium deoxidized steel was mainly composed of Zr, O and a small amount of Al by SEM-EDS method. Based on the stoichiometric relationship between zirconium oxide and aluminum oxide, the inclusion was analyzed to be composed of 94% ZrO₂ and 6% Al₂O₃. The inclusion size distribution in zirconium deoxidized steel is normal. The average inclusion size is 0.62 μm, and the number of inclusions is the largest in the range of 0.7~0.8 μm. The three-dimensional morphology of non-metallic inclusions in steel can be observed using SEM combined with electrolysis. The EDS method can be used to qualitatively analyze the composition and distribution of elements in inclusions individually. The composition of inclusions with single valence can be quantitatively analyzed. However, for non-metallic inclusions with many valence states and unknown valence states, the EDS method alone cannot accurately analyze the phase and composition of inclusions. The presence of monoclinic zirconia in zirconium-deoxidized steel was detected by Raman spectroscopy combined with electrolysis extraction of inclusions. TEM diffraction pattern calibration and energy spectrum analysis of a single inclusion detected Zirconia with monoclinic phase. Two phases, including monoclinic and tetragonal zirconia, were detected by μXRD combined with electrolytic extraction of inclusions, and the lattice parameters of zirconia inclusions were obtained. These three methods detected no aluminum-containing phase. Raman spectroscopy, TEM and μXRD can be used to qualitatively analyze the phase and composition of inclusions after electrolytic extraction, but the three methods cannot accurately characterize the phase with low content. TEM and μXRD can characterize the crystal structure and lattice parameters of the inclusion. TEM and SEM can only characterize individual inclusions one by one. μXRD and Raman spectroscopy can characterize the phase of all the inclusions in the detected region, a statistically significant method to characterize inclusions. Therefore, the inclusion characteristics can be characterized comprehensively and accurately by SEM-EDS analysis combined with μXRD analysis.

Key words：Non-metallic inclusion; SEM-EDS; Raman spectroscopy; TEM; μXRD

Received: 2022-08-29 Accepted: 2023-06-05

ZTFLH:

TF701.3

Corresponding Authors: WANG Lin-zhu E-mail: lzwang@gzu.edu.cn

Cite this article:

LI Yu-tang,WANG Lin-zhu,LI Xiang, et al. Characterization and Comparative Analysis of Non-Metallic Inclusions in Zirconium Deoxidized Steel[J]. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2023, 43(09): 2916-2921.

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https://www.gpxygpfx.com/EN/10.3964/j.issn.1000-0593(2023)09-2916-06 OR https://www.gpxygpfx.com/EN/Y2023/V43/I09/2916

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