Evaluation of Sulfide Inclusions before and after Deformation of Steel by Using the Electrolytic Extraction Method

The characteristics of elongated MnS have a critical effect on fatigue anisotropy and all mechanical anisotropies. A comparative investigation of nonmetallic inclusions in both stainless steels and tool steels has been carried out in this study. The inclusion characteristics were investigated using electrolytic extraction (EE) followed by scanning electron microscopy combined with energy-dispersive spectroscopy (SEM-EDS). Overall, three types of MnS inclusions (type I (regular), type II (irregular) and type III (Rod)) were found in tool steels in as-cast samples, which had not been heat-treated. Furthermore, three types of MnS inclusions (Rod-like sulfide (RS), Plate-like sulfide (PS) and Oxysulfide (OS)) were found in samples taken after rolling. Based on the breakability of the elongated MnS, three types of inclusions, Type UU, UB and BB, where U represents the undamaged or unbroken edge of an inclusion and B represents the fragment or broken edge of an inclusion, were studied in both stainless steels and tool steels both before and after additional heat treatment. The effect of heat treatment and dissolving the metal layer during the EE process is also discussed. The results show that both processes have a limited effect on the breakability of inclusions in steels with carbon contents <0.42 mass%.

Application of Some Modern Analytical Techniques for Characterization of Non-Metallic Inclusions in a Fe-10mass%Ni Alloy Deoxidized by Ti/Zr and Ti/Mg

In this study, a complete and comprehensive analysis of non-metallic inclusions (NMI) in an Fe-10%Ni alloy was done by using two modern analytical methods that complement each other: Electrolytic Extraction (EE) of inclusions from metal samples followed by investigations by using Scanning Electron Microscopy (SEM) and Fractional Gas Analysis (FGA). The composition, morphology, size and number of different NMIs and clusters were investigated in metal samples taken after deoxidation by additions of Ti, Ti/Zr and Ti/Mg. The obtained results were discussed with respect to formation, modification and removal of NMIs and clusters depending on the type of deoxidations and the holding time. It was found that the peaks of oxygen reduced from different oxide inclusions obtained by the FGA measurements corresponded well to the main types of inclusions and clusters observed by using the EE + SEM method. More specifically, the total O content in oxide inclusions (ONMI) increases by 10% after a Zr addition and then decreases linearly by 40% during 5 min of holding due to flotation of NMIs and clusters. However, after a Mg addition in the melt deoxidized by Ti, the ONMI content decreases drastically by 63% during 5 min of holding, due to a fast floatation of NMIs caused by bubbles of vaporized Mg.

Origin of the Inclusions in Production-Scale Electrodes, ESR Ingots, and PESR Ingots in a Martensitic Stainless Steel

The focus of the study was to define the origin of the inclusions in production-scale electro-slag remelting, (ESR) and electro-slag remelting under a protected pressure controlled atmosphere, (PESR), ingots. The inclusion characteristics in production samples were studied using both polished sample surfaces (two-dimensional (2-D) investigations) and inclusions extracted from steel samples by electrolytic extraction (three-dimensional (3-D) investigations) using SEM in combination with EDS. The results were compared to results from previously reported laboratory-, pilot-, and production-scale trials including electrode, remelted, and conventional ingots. The results show that primary, semi-secondary, and secondary inclusions exist in the remelted ingots. The most probable inclusion to survive from the electrode is a MgO-Al2O3 (spinel). It was also found that the ESR/PESR process slag acts in a similar way to a calcium treatment modification of alumina inclusions. On the whole, the most significant finding is that the overall cleanliness of the electrode including the inclusions in the electrode has an influence on the inclusion content of the ESR and PESR ingots.

The Three-Dimensional Morphology and Distribution of CaS Inclusions in Continuous Casting Slab of Ni20Mn6 Steel

Calcium sulfide (CaS) inclusion with large and irregular shape is detrimental to the properties of steel. Understanding the shape and distribution of CaS inclusions in a continuous casting (CC) slab is of significance for improving the rolling properties. In this study, CaS inclusions were extracted from CC slab of Ni20Mn6 steel using the electrolytic extraction and investigated by scanning electron microscopy (SEM)-energy dispersive X-ray spectroscopy (EDX). The CaS inclusions morphologies vary with their locations in the CC slab and, thus, are classified into five categories. The thermodynamics calculated results showed that CaS inclusions precipitated at the end of solidification due to the microsegregation of sulfur and calcium in the interdendrite liquid and finally precipitated along the austenite grain boundary. The macrosegregation degree of solutes in different regions is one of the reasons that affect the size of CaS inclusion. The morphologies of CaS inclusion are affected by the solidification structure of slab and austenite grain boundary.

Effect of Inclusions on the Corrosion Properties of the Nickel-Based Alloys 718 and EP718

Inclusions in steels and alloys are known to lower the resistance to deformation, as well as to lower the mechanical, corrosion and other properties. Studies of inclusions in nickel-based alloys are important since these materials could suffer from corrosion degradation in harsh operational conditions. This, in fact, could lead to a pitting initiation around the inclusions. Two industrial Ni-based alloys (alloy 718 and EP718) were investigated to determine the harmful effects of different inclusions on the corrosion resistance of Ni-based alloys. Specifically, the inclusion characteristics (such as composition, morphology, size, number and location) were determined for inclusions collected on film filters after electrolytic extraction and dissolution of a metal matrix around different inclusions on surfaces of metal samples after electrolytic extraction (EE). It was found that both Ni-based alloys contain various inclusion types: carbides (large size NbTi-C and small multicomponent carbides), nitrides TiNb-N and sulphides (TiNb-S in EP718 alloy). The most harmful effects on the corrosion resistance of metal were detected around sulphides and small carbides containing Mo, W, Cr. Dissolution effects were also observed around large carbides and nitrides, especially around inclusions larger than 10 µm. Moreover, the dissolution of a matrix around inclusions and clusters located on the grain boundaries were found to be 2.1–2.7 times larger compared to inclusions found inside of grains of the given alloy samples.

Effect of Inclusions on the Corrosion Properties of Nickel Based Alloys 718 and EP718

Inclusions in steels and alloys are known as factors that could lower deformation, mechanical, corrosion and other properties. Study of inclusions in nickel based alloys is important since these materials could suffer from corrosion degradation in harsh operational conditions, where inclusions could lead to a pitting initiation. For estimation of a harmful effect of different inclusions on corrosion resistance of Ni-based alloys, inclusion characteristics (such as composition, morphology, size, number and location) on film filter and dissolution of metal matrix around different inclusions on surfaces of metal samples after electrolytic extraction (EE) were investigated in two samples of industrial Ni-based alloys (alloy 718 and EP718). It was found that both Ni-based alloys have various inclusions: carbides (large size NbTi-C and small multicomponent carbides), nitrides TiNb-N and sulfides (TiNb-S in EP718 alloy). The higher harmful effect on corrosion resistance of metal was detected around sulfides and small carbides containing Mo, W, Cr. Dissolution effect was also observed around large carbides and nitrides, especially around inclusions having size more than 10 &micro;m. Moreover, the dissolution of metal matrix around inclusions and clusters located on the grain boundaries is 2.1-2.7 times larger compared to that for those inclusions inside of grains of the given alloy samples.

Study on the Possible Error Due to Matrix Interaction in Automated SEM/EDS Analysis of Nonmetallic Inclusions in Steel by Thermodynamics, Kinetics and Electrolytic Extraction

Up to now, the Fe content of nonmetallic particles has often been neglected in chemical evaluations due to the challenging analysis of matrix elements in nonmetallic inclusions (NMI) in steel by scanning electron microscope and energy dispersive spectroscopy analysis (SEM/EDS). Neglecting matrix elements as possible bonding partners of forming particles may lead to inaccurate results. In the present study, a referencing method for the iron content in nonmetallic inclusions in the submicrometer region is described focusing on the system Fe-Mn-O. Thermodynamic and kinetic calculations are applied to predict the inclusion population for different Fe/Mn ratios. Reference samples containing (Fe,Mn)-oxide inclusions with varying Fe ratios are produced by manganese deoxidation in a high-frequency induction furnace. Subsequent SEM/EDS measurements are performed on metallographic specimens and electrolytically extracted nonmetallic inclusions down to 0.3 µm. The limits of iron detection in these particles, especially for those in the submicrometric regime, as well as the possible influence of electrolytic extraction on Fe-containing oxide particles are examined. The measured inclusion compositions correlate well with the calculated results regarding segregation and kinetics. The examinations performed are reliable proof for the application of SEM/EDS measurements to evaluate the Fe content in nonmetallic inclusions, within the physical limits of polished cross-section samples. Only electrolytic extraction ensures the determination of accurate compositions of dissolved or bonded matrix elements at smallest particles enabling quantitative particle descriptions for submicrometric (particles ≤ 1 µm) steel cleanness evaluations.

Transient Evolution of Inclusions during Al and Ti Additions in Fe-20 Mass pct Cr Alloy

The transient evolution of inclusions during Al and Ti additions in a Fe-20 mass pct Cr alloy was investigated using polished cross sections and electrolytic extraction. After Al addition, the evolution of Al2O3-based inclusions based upon the area and particle size passed through the following three main stages with time: Particle agglomeration, inclusion floating, and a slow decrease of the remaining Al2O3-based inclusions. Titanium wire was fed into the steel at the end of the floating stage after Al addition when the Ostwald ripening process was finished. Immediately after Ti addition, the transient phase of Ti oxide was readily generated on the existing Al2O3-based inclusion and disappeared due to Al reduction as time progressed. The formation of the transient TiOx phase was affected by the low disregistry between Al2O3 and TiOx and the local Ti supersaturation, which cannot be predicted by the equilibrium relations of Ti–O–N or Ti–Al–O in the high-Cr-containing melt. Because of the local supersaturation of dissolved [%Ti] and [%N] shortly after Ti addition, TiN associated with existing inclusions and three types of individual TiN including single cubes, twinned inclusions, and clusters were identified. In order to minimize the Ti loss caused by the formation of Ti-rich zones during the transient stages, the removal of large Al2O3-based particles including aggregates, clusters, and flower-shaped inclusions should be promoted by stirring before Ti addition. After Ti addition, Brownian and turbulent were the major factors affecting the collision of particles smaller than the threshold of 2.7 μm. The agglomeration of inclusions larger than this threshold was mainly dominated by turbulent and Stokes’ collisions.

An Investigation of Non-Metallic Inclusions in Different Ferroalloys using Electrolytic Extraction

Ferroalloys are integral constituents of the steelmaking process, since non-metallic inclusions (NMIs) from ferroalloys significantly influence the transformation of inclusions present in liquid steel or they are directly involved in casted steel. In this study, the characteristics of inclusions (such as the number, morphology, size, and composition) in different industrial ferroalloys (FeV, FeMo, FeB, and FeCr) were investigated using the electrolytic extraction (EE) technique. After extraction from the ferroalloy samples and filtration of the solution, the inclusions were investigated on a film filter. The three-dimensional (3D) investigations were conducted using a scanning electron microscopy in combination with energy dispersive spectroscopy (SEM-EDS). The characteristics of inclusions observed in the ferroalloys were compared with previous results and discussed with respect to their possible behaviors in the melt and their effects on the quality of the cast steels. The particle size distributions and floatation distances were plotted for the main inclusion types. The results showed that the most harmful inclusions in the ferroalloys investigated are the following: pure Al2O3 and high Al2O3-containing inclusions in FeV alloys; pure SiO2 and high SiO2-containing inclusions in FeMo alloys; Al2O3 and SiO2-containing inclusions in FeB alloys; and MnO-Cr2O3, Al2O3, and Cr2O3-based inclusions in FeCr alloys.