Effect of magnesium addition on inclusions in H13 die steel

The effect of magnesium addition on the number, morphology, composition, size, and density of inclusions in H13 die steel was studied. The results show that the total oxygen content in the steel can be significantly decreased to 0.0008wt%. Al₂O₃ and MnS inclusions are changed into nearly spherical MgO·Al₂O₃ spinel and spherical MgO·MgS inclusions, respectively. The number of inclusions larger than 1 μm decreases and the number of inclusions smaller than 1 μm increases with increasing magnesium content. V(N,C) precipitates around MgO·Al₂O₃ and MgO·MgS inclusions during solidification of liquid steel. The densities of MgO·Al₂O₃ spinel inclusions are lower than that of alumina inclusions. With increasing magnesium content in the Mg-containing inclusions, the density of inclusions decreases, leading to the improvement of inclusion removal efficiency.     

Development of inclusions in 3104 alloy melt during heating and holding treatments

Developments in the contents of different typical inclusions in 3104 alloy melt were described during heating and holding processing. The settling process of inclusion particles was investigated by measuring the contents of inclusions in the surface, center, and bottom layers of the molten metal. In the results, main inclusions observed and determined by Prefil and PoDFA methods are MgO, Al₂O₃, spinel (MgAl₂O₄), and TiB₂ particles or thin films. It is found that some small particles of Al₂O₃ and MgO are transformed into spinel particles, and the formation rate increases as the temperature and the holding period of melt increase. The content of inclusions increases from 3.37 mm2·kg-1 to 7.54 mm2·kg-1 and then decreases to 3.08 mm2·kg-1 after holding for 90 min. This is attributed to a settling phenomenon and a significant increase in settling velocity after holding for 60 min. The content of inclusion particles decreases by means of settlement and flotation in liquid aluminum with an increase in holding time. The theoretical analysis and experiment results are in essential agreement with those from industrial production.     

18wt%Cr–8wt%Ni不锈钢中增塑性MnO–Al2O3–SiO2基非金属夹杂物的演变及其浸泡性能

The properties of MnO–Al₂O₃–SiO₂-based plasticized inclusion are likely to change during soaking  process due to its low melting point. In this study, the evolution of the MnO–Al₂O₃–SiO₂-based inclusion of 18wt%Cr?8wt%Ni stainless steel under isothermal soaking process at 1250°C for different times was investigated by laboratory-scale experiments and thermodynamic analysis. The results showed that the inclusion population density increased at the first stage and then decreased while their average size first decreased and then increased. In addition, almost no Cr₂O₃-concentrated regions existed within the inclusion before soaking, but more and more Cr₂O₃ precipitates were formed during soaking. Furthermore, the plasticity of the inclusion deteriorated due to a decrease in the amount of liquid phase and an increase in the high-melting-point-phase MnO–Cr₂O₃ spinel after the soaking process. In-situ observations by high-temperature confocal laser scanning microscopy (CLSM) confirmed that liquid phases were produced in the inclusions and the inclusions grew rather quickly during the soaking process. Both the experimental results and thermodynamic analysis conclude that there are three routes for inclusion evolution during the soaking process. In particular, Ostwald ripening plays an important role in the inclusion evolution, i.e., MnO–Al₂O₃–SiO₂-based inclusions grow by absorbing the newly precipitated smaller-size MnO–Cr₂O₃ inclusions.     

Comparison between the surface defects caused by Al2O3 and TiN inclusions in interstitial-free steel auto sheets

Al₂O₃ and TiN inclusions in interstitial-free (IF) steel deteriorate the properties of the steel. To decrease the defects of cold-rolled sheet, it is important to clearly distinguish between the degrees of damage caused by these two inclusions on the surface quality of the steel. In this study, a nanoindenter was used to test the mechanical properties of the inclusions, and the distribution and size of the inclusions were obtained by scanning electron microscopy (SEM). It was found that when only mechanical properties are considered, TiN inclusions are more likely to cause defects than Al₂O₃ inclusions of the same size during the rolling process. However, Al₂O₃ inclusions are generally more inclined to cause defects in the rolling process than TiN inclusions because of their distribution characteristic in the thickness direction. The precipitation of Al₂O₃ and TiN was obtained through thermodynamical calculations. The growth laws of inclusions at different cooling rates were calculated by solidification and segregation models. The results show that the precipitation regularity is closely related to the distribution law of the inclusions in IF slabs along the thickness direction.     

Novel mechanism for the modification of Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-based inclusions in ultra-low carbon Al-killed steel considering the effects of magnesium and calcium

Many researchers have explored the inclusion modification mechanism to improve non-metallic inclusion modifications in steelmaking. In this study, two types of industrial trials on inclusion modifications in liquid steel were conducted using ultra-low-carbon Al-killed steel with different Mg and Ca contents to verify the effects of Ca and Mg contents on the modification mechanism of Al₂O₃-based inclusions during secondary refining. The results showed that Al₂O₃-based inclusions can be modified into liquid calcium aluminate or a multi-component inclusion with the addition of a suitable amount of Ca. In addition,[Mg] in liquid steel can further reduce CaO in liquid calcium aluminate to drive its evolution into CaO-MgO-Al₂O₃ multi-component inclusions. Thermodynamic analysis confirmed that the reaction between[Mg] and CaO in liquid calcium aluminate occurs when the MgO content of liquid calcium aluminate is less than 3wt% and the temperature is higher than 1843 K.     

Effect of Ce on the cleanliness,microstructure and mechanical properties of high strength low alloy steel Q690E in industrial production process

In order to improve the strength and toughness of Q690E steel sheets, the effect of rare earth element Ce on the strength and toughness of Q690E steel was studied by means of transmission electron microscopy, scanning electron microscopy, and metallographic microscope. The results showed that the addition of Ce in steel limited the combination of S with Mn and Ca, transformed Al₂O₃ inclusion into spherical CeAlO₃ inclusion, and modified the precipitate form of some composite inclusions of TiN and sulfide oxides into TiN precipitation alone. The inclusions were spheroidizing. The size of inclusions was decreased from 3-5 μm to 1-2 μm, and the distribution was dispersed. Ce played a role in purifying molten steel through desulphurization and deoxidization. Meanwhile, the addition of Ce in steel effectively increased the nucleation particles in the liquid phase, improved the nucleation rate, enlarged the equiaxed grain refinement area, and limited the development of columnar crystals. The average grain size of slab decreased from 45.76 to 35.25 μm, and the proportion of large grain size (> 50 μm) decreased from 40.41% to 23.74%. The macrostructural examination of slab was improved from B0.5 to C2.0, which realized the refinement of the solidified structure and reduced the banded structure of hot rolled plate. In addition, due to the inheritance of refined structure in the upstream, the recrystallization of deformed austenite and the growth of grain after recrystallization were restrained, and a refined tempered sorbite structure was obtained. When rare earth element Ce was added, the width of the martensite lath bundle was narrowed from about 500 nm to about 200 nm, which realized a remarkable grain refinement strengthening and toughening effect. Mechanical properties such as tensile, yield, and low-temperature impact toughness were significantly improved.     

SEM In-situ Observation at Tensile Loading on Surface Inclusion in PM Rene95 Superalloy

The observation on crack initiation and propagation of surface inclusion Al₂O₃ in seeded PM Rene95 was conducted by SEM in-situ tension test. The results show that the cracks often initiate at the inclusion/matrix interface vertical to the applied stress direction, and easily propagate along the interface into the matrix. The interface of inclusion/matrix is just mechanically bounded on the base of SEM observation. The weak bonding of inclusion/matrix interface and stress concentration around inclusions are the main reasons of the matrix/inclusion interface debonding and local plastic deformation under the tensile loading in the in-situ tension test. Surface inclusion does not definitely lead to the failure of in-situ tension test. But the early surface crack initiation caused by ceramic inclusion is critically harmful to the LCF property of PM Rene95 superalloy, which can't be ignored.     

Determination of inclusions in liquid steel after calcium treatment

Nozzle blocking was eliminated by calcium-treated liquid steel through changing the chemical and phase composition of alumina inclusions in aluminium-killed steel. Three different methods were applied to determine the composition of inclusions in liquid steel: total oxygen content samples, sampling spoon samples, and “lollipop” steel samples. The results show that calcium modification of liquid steel influences the inclusion composition varying from 2wt% to 14wt% depending on the method used. The composition of inclusions contains mainly Al₂O₃-CaO only, or is associated with SiO₂ or MgO depending on the initial input. The methods used in this study are indicators of the inclusion composition but can be improved to quantify the inclusion size.     

Characteristics of Al<Subscript>2</Subscript>O<Subscript>3</Subscript>, MnS,and TiN inclusions in the remelting process of bearing steel

The Al₂O₃, MnS, and TiN inclusions in bearing steel will deteriorate the steel's mechanical properties. Therefore, elucidating detailed characteristics of these inclusions in consumable electrode during the electroslag remelting process is important for achieving a subsequently clean ingot. In this study, a confocal scanning violet laser microscope was used to simulate the remelting process and observe, in real time, the behaviors of inclusions. The obtained images show that, after the temperature exceeded the steel solidus temperature, MnS and TiN inclusions in the specimen began to dissolve. Higher temperatures led to faster dissolution, and the inclusions disappeared before the steel was fully liquid. In the case of an observed Al₂O₃ inclusion, its shape changed from angular to a smooth ellipsoid in the region where the solid and liquid coexisted and it began to dissolve as the temperature continued to increase. This dissolution was driven by the difference in oxygen potential between the inclusion and the liquid steel.     

Effect of interaction of refractories with Ni-based superalloy on inclusions during vacuum induction melting

This study documents laboratory-scale observation of the interactions between the Ni-based superalloy FGH4096 and refractories. Three different crucibles were tested—MgO, Al₂O₃, and MgO–spinel. We studied the variations in the compositions of the inclusions and the alloy–crucible interface with the reaction time using scanning electron microscopy equipped with energy dispersive X-ray spectroscopy and X-ray diffraction. The results showed that the MgO and MgO–spinel crucibles form MgO-containing inclusions (Al–Mg oxides and Al–Mg–Ti oxides), whereas the inclusions formed when using the Al₂O₃ crucible are Al₂O₃ and Al–Ti oxides. We observed a new MgAl₂O₄ phase at the inner wall of the MgO crucible, with the alloy melted in the MgO crucible exhibiting fewer inclusions. No new phase occurred at the inner wall of the Al₂O₃ crucible. We discuss the mechanism of interaction between the refractories and the Ni-based superalloy. Physical erosion was found to predominate in the Al₂O₃ crucible, whereas dissolution and chemical reactions dominated in the MgO crucible. No reaction was observed between three crucibles and the Ti of the melt although the Ti content (3.8wt%) was higher than that of Al (2.1wt%).     

Effect of Al content on the reaction between Fe-10Mn-xAl(x=0.035wt%,0.5wt%,1wt%,and 2wt%)steel and CaO-SiO2-Al2O3-MgO slag

The effect of Al content(0.035 wt%,0.5 wt%,1 wt%,and 2 wt%)on the composition change of steel and slag as well as inclusion transformation of high manganese steel after it has equilibrated with Ca O-Si O₂-Al₂O₃-Mg O slag was studied using the method of slag/steel reaction.The experimental results showed that as the initial content of Al increased from 0.035 wt%to 2 wt%,Al gradually replaced Mn to react with Si O₂in slag to avoid the loss of Mn due to the reaction;this process caused both Al₂O₃in slag and Si in steel to increase while Si O₂and Mn O in slag to reduce.In addition,the type of inclusions also evolved as the initial Al content increased.The evolution route of inclusions was Mn O→Mn O-Al₂O₃-Mg O→Mg O→Mn O-Ca O-Al₂O₃-Mg O and Mn O-Ca O-Mg O.The shape of inclusions evolved from spherical to irregular,became faceted,and finally transformed to spherical.The average size of inclusions presented a trend that was increasing first and then decreasing.The transformation mechanism of inclusions was explored.As the initial content of Al increased,Mg and Ca were reduced from top slag into molten steel in sequence,which consequently caused the transformation of inclusions.     

Desulfurization ability of refining slag with medium basicity

The desulfurization ability of refining slag with relative lower basicity (B) and Al₂O₃ content (B = 3.5–5.0; 20wt%–25wt% Al₂O₃) was studied. Firstly, the component activities and sulfide capacity (C_S) of the slag were calculated. Then slag-metal equilibrium experiments were carried out to measure the equilibrium sulfur distribution (L_S). Based on the laboratorial experiments, slag composition was optimized for a better desulfurization ability, which was verified by industrial trials in a steel plant. The obtained results indicated that an MgO-saturated CaO-Al₂O₃-SiO₂-MgO system with the basicity of about 3.5–5.0 and the Al₂O₃ content in the range of 20wt%–25wt% has high activity of CaO (a_CaO), with no deterioration of C_S compared with conventional desulfurization slag. The measured L_S between high-strength low-alloyed (HSLA) steel and slag with a basicity of about 3.5 and an Al₂O₃ content of about 20wt% and between HSLA steel and slag with a basicity of about 5.0 and an Al₂O₃ content of about 25wt% is 350 and 275, respectively. The new slag with a basicity of about 3.5–5.0 and an Al₂O₃ content of about 20wt% has strong desulfurization ability. In particular, the key for high-efficiency desulfurization is to keep oxygen potential in the reaction system as low as possible, which was also verified by industrial trials.     

Nonmetallic inclusions in SUS304 strip produced by twin-roll strip casting

The shape, type, content, and dimension of nonmetallic inclusions in SUS304 strip produced by twin-roll strip casting were studied using scanning electron microscopy (SEM). The results show that the inclusions are mainly spherical Al₂O₃ and complex oxides composed of MnO, Al₂O₃, and SiO₂. The percentage of fine oxides smaller than 3 μm reaches up to 51.8%. The theoretical calculations show that fine oxides have precipitated during solidification. Therefore, it is concluded that during twin-roll strip casting, because of high cooling rate, the size of inclusions precipitated during solidification decreases, and the amount increases.     

Inclusion variations and calcium treatment optimization in pipeline steel production

SiCa line and SiCaBaFe alloy were injected into liquid pipeline steel at the end of LF refining as calcium treatment, and samples were taken from the ladles, mould, and slabs. Analysis of Ca content and inclusions shows that Ca content in steel decreases obviously in the following process after calcium treatment; the compositions, morphology, and sizes of inclusions also vary much in the production; primary inclusions in the ladles prior to calcium treatment are mainly Al₂O₃ inclusions, but they turn to fine irregular CaS-CaO-Al₂O₃ compound inclusions after the treatment, then become fine globular CaO-Al₂O₃ inclusions in the mould, and finally change to a few larger irregular CaS-CaO-Al₂O₃ complex inclusions in the slabs. Thermodynamic study reveals that inclusion variations are related with the preferential reactions among Ca, Al₂O₃, and S and the precipitation of S in CaO-Al₂O₃ inclusions with high sulfur capacity. New evaluation standards for calcium treatment in high-grade pipeline steel were put forward according to the inclusion variations and requirements of pipeline steel on inclusion controlling, and the calcium process was studied and optimized.     

Numerical simulation on inclusion transport in continuous casting mold

Turbulent flow, the transport of inclusions and bubbles, and inclusion removal by fluid flow transport and by bubble flotation in the strand of the continuous slab caster are investigated using computational models, and validated through comparison with plant measurements of inclusions. Steady 3-D flow of steel in the liquid pool in the mold and upper strand is simulated with a finite-difference computational model using the standard k-ε turbulence model. Trajectories of inclusions and bubbles are calculated by integrating each local velocity, considering its drag and buoyancy forces. A “random walk” model is used to incorporate the effect of turbulent fluctuations on the particle motion. The attachment probability of inclusions on a bubble surface is investigated based on fundamental fluid flow simulations, incorporating the turbulent inclusion trajectory and sliding time of each individual inclusion along the bubble surface as a function of particle and bubble size. The change in inclusion distribution due to removal by bubble transport in the mold is calculated based on the computed attachment probability of inclusions on each bubble and the computed path length of the bubbles. The results indicate that 6%-10% inclusions are removed by fluid flow transport, 10% by bubble flotation, and 4% by entrapment to the submerged entry nozzle (SEN) walls. Smaller bubbles and larger inclusions have larger attachment probabilities. Smaller bubbles are more efficient for inclusion removal by bubble flotation, so long as they are not entrapped in the solidifying shell. A larger gas flow rate favors inclusion removal by bubble flotation. The optimum bubble size should be 2-4 mm.     

Occurrence mechanism of silicate and aluminosilicate minerals in Sarcheshmeh copper flotation concentrate

The Sarcheshmeh copper flotation circuit is producing 5×104 t copper concentrate per month with an averaging grade of 28% Cu in rougher, cleaner and recleaner stages. In recent years, with the increase in the open pit depth, the content of aluminosilicate minerals increased in plant feed and subsequently in flotation concentrate. It can motivate some problems, such as unwanted consumption of reagents, decreasing of the copper concentrate grade, increasing of Al₂O₃ and SiO₂ in the copper concentrate, and needing a higher temperature in the smelting process. The evaluation of the composite samples related to the most critical working period of the plant shows that quartz, illite, biotite, chlorite, orthoclase, albeit, muscovite, and kaolinite are the major Al₂O₃ and SiO₂ beating minerals that accompany chalcopyrite, chalcocite, and covellite minerals in the plant feed. The severe alteration to clay minerals was a general rule in all thin sections that were prepared from the plant feed. Sieve analysis of the flotation concentrate shows that Al₂O₃ and SiO₂ bearing minerals in the flotation concentrate can be decreased by promoting the size reduction from 53 to 38 μm. Interlocking of the Al₂O₃ and SiO₂ bearing minerals with chalcopyrite and chalcocite is the occurrence mechanism of silicate and aluminosilicate minerals in the flotation concentrate. The dispersed form of interlocking is predominant.     

Subsurface macro-inclusions and solidified hook character in aluminum-killed deep-drawing steel slabs

Subsurface macro-inclusions and hooks are detrimental to the surface quality of deep-drawing steel sheets. However, little is known about the relationship between macro-inclusions and hooks. Thus, in this work, two ultralow carbon (ULC) steel slabs and two low carbon (LC) aluminum-killed steel slabs were sampled to study the relationship between hooks and subsurface macro-inclusions, which were detected on the cross-sections of steel samples with an area of 56058 mm2 using an automated scanning electron microscopy/energy-dispersive X-ray spectroscopy system. Results show that subsurface inclusions larger than 200 μm were almost entrapped by hook structures, whereas the location of other inclusions smaller than 200 μm had no obvious dependence on the location of solidified hooks. Furthermore, the number density (ND) of subsurface inclusions larger than 200 μm decreased from 0.02 to 0 cm-2 in ULC steel as the mean hook depth decreased from 1.57 to 1.01 mm. Similar trends were also observed in LC steel. In addition, the detected inclusions larger than 200 μm were concentrated in the region near the slab center (3/8 width-5/8 width), where hook depths were also larger than those at any other locations. Therefore, minimizing the hook depth is an effective way to reduce inclusion-induced sliver defects in deep-drawing steels.     

Activity coefficient of NiO in SiO2-saturated MnO–SiO2slag and Al2O3-saturated MnO–SiO2–Al2O3slag at 1623 K

As a part of the fundamental study related to the reduction smelting of spent lithium-ion batteries and ocean polymetallic nodules based on MnO–SiO₂slags,this work investigated the activity coefficient of NiO in SiO₂-saturated Mn O–Si O₂slag and Al₂O₃-saturated Mn O–SiO₂–Al₂O₃slag at 1623 K with controlled oxygen partial pressure levels of 10^-7,10^-6,and 10^-5Pa.Results showed that the solubility of nickel oxide in the slags increased with increasing oxygen partial pressure.The nickel in the Mn O–Si O₂slag and Mn O–Si O₂–Al₂O₃slag existed as Ni O under experimental conditions.The addition of Al₂O₃in the Mn O–Si O₂slag decreased the dissolution of nickel in the slag and increased the activity coefficient of Ni O.Furthermore,the activity coefficient of Ni O(γN_(i O)),which is solid Ni O,in the Si O₂saturated Mn O–Si O₂slag and Al₂O₃saturated Mn O–Si O₂–Al₂O₃slag at 1623 K can be respectively calculated asγN_(i O)=8.58w(Ni O)+3.18 andγN_(i O)=11.06w(Ni O)+4.07,respectively,where w(Ni O)is the Ni O mass fraction in the slag.     

Novel mechanism for the modification of Al_2O_3-based inclusions in ultra-low carbon Al-killed steel considering the effects of magnesium and calcium

Many researchers have explored the inclusion modification mechanism to improve non-metallic inclusion modifications in steelmaking. In this study, two types of industrial trials on inclusion modifications in liquid steel were conducted using ultra-low-carbon Al-killed steel with different Mg and Ca contents to verify the effects of Ca and Mg contents on the modification mechanism of Al_2O_3-based inclusions during secondary refining. The results showed that Al_2O_3-based inclusions can be modified into liquid calcium aluminate or a multi-component inclusion with the addition of a suitable amount of Ca. In addition, [Mg] in liquid steel can further reduce CaO in liquid calcium aluminate to drive its evolution into CaO–MgO–Al_2O_3 multi-component inclusions. Thermodynamic analysis confirmed that the reaction between [Mg] and CaO in liquid calcium aluminate occurs when the MgO content of liquid calcium aluminate is less than 3 wt% and the temperature is higher than 1843 K.     

原位纳米增强高强韧钢氢脆性能研究

We investigated the critical influence of in-situ nanoparticles on the mechanical properties and hydrogen embrittlement (HE) of high-strength steel. The results reveal that the mechanical strength and elongation of quenched and tempered steel (919 MPa yield strength, 17.11% elongation) are greater than those of hot-rolled steel (690 MPa yield strength, 16.81% elongation) due to the strengthening effect of in-situ Ti₃O₅–Nb(C,N) nanoparticles. In addition, the HE susceptibility is substantially mitigated to 55.52%, approximately 30% lower than that of steels without in-situ nanoparticles (84.04%), which we attribute to the heterogeneous nucleation of the Ti₃O₅ nanoparticles increasing the density of the carbides. Compared with hard TiN inclusions, the spherical and soft Al₂O₃–MnS core–shell inclusions that nucleate on in-situ Al₂O₃ particles could also suppress HE. In-situ nanoparticles generated by the regional trace-element supply have strong potential for the development of high-strength and hydrogen-resistant steels.