Theory and Practice of Oxide Inclusion Composition and Morphology Control in Spring Steel Production

In order to control the composition,morphology and size distribution of oxide inclusions in spring steel,the relationship between the content or activity of aluminum and calcium in molten steel and compositions of oxide inclusion precipitated at different temperatures was determined based on thermodynamic equilibrium for spring steel 60Si2 MnA,and has been verified by practice.The size distribution of non-metallic inclusions electrolytically extracted from specimens of hot rolled spring steel was determined by image analyzer.The results show that there are a great deal of large inclusions in spring steel produced by the conventional process,and the quantity and the size of large inclusions in spring steel produced by new process are largely reduced.As a result,the fatigue properties of the spring steel produced by new process are highly improved,and the ratio ofσ-1/σbis raised from 0.451 to 0.468.

Temperature-dependent evolution of oxide inclusions during heat treatment of stainless steel with yttrium addition

The evolution of oxide inclusions during isothermal heating of 18Cr–8Ni stainless steel with yttrium addition at temperatures of 1273 to 1573 K was investigated systematically.Homogeneous spherical Al–Y–Si(–Mn–Cr)oxide inclusions were observed in as-cast steel.After heating,most of the homogeneous inclusions were transformed into heterogeneous inclusions with Y-rich and Al-rich parts,even though some homogeneous oxide particles were still observed at 1273 and 1573 K.With the increase in heating temperature,more large-sized inclusions were formed.The shape of the inclusions also changed from spherical to irregular.The maximum transformation temperature of inclusions was determined to be 1373 K.The evolution mechanism of inclusions during heating was proposed to be the combined effect of the(i)internal transformation of inclusions due to the crystallization of glassy oxide and(ii)interfacial reaction between inclusions and steel matrix.Meanwhile,the internal transformation of inclusions was considered to be the main factor at heating temperatures less than 1473 K.

Cerium oxide inclusion nucleation mechanism based on classical nucleation theory and two-step nucleation

It is challenging to assess the mechanism responsible for the nucleation of inclusions in metals at high temperatures.The present work therefore systematically investigates the nucleation of cerium oxide inclusions according to classical nucleation theory and a two-step nucleation mechanism.The nucleation rates and nucleation radii of these inclusions are obtained,and the results demonstrate a considerable difference between theoretical and experimental values.On the basis of a two-step nucleation mechanism,(CeO_(2))_(n) and(Ce_(2)O_(3))_(n)(n=1-6)clusters were constructed and the thermodynamic properties of both these clusters and of cerium oxide nanoparticles were analyzed.In addition,the entropies and heat capacity changes of cerium oxides were determined using first principles calculations and are found to be consistent with literature data.The present data indicate that the cerium oxide inclusion nucleation pathway can be summarized as[Ce]+[O]→(CeO_(2))n/(Ce_(2)O_(3))_(n)→(Ce_(2)O_(3))_(n)→(Ce_(2)O_(3))_(2)→core(Ce_(2)O_(3)crystal)-shell((Ce_(2)O_(3))_(2) cluster)nanoparticles→(Ce_(2)O_(3))bulk.

Effect of oxide inclusions on MnS precipitates and tensile mechanical property of high-strength low-alloy steel

The key role of oxide inclusions on the microstructure and mechanical property of a high-strength low-alloy steel was investigated.The field emission scanning electron microscope equipped with energy-dispersive spectrometry was used to characterize MnS precipitates.Oxide inclusions play an important role in the shape control of MnS precipitates.More oxides fovored to decrease the size and the aspect ratio of MnS precipitates.With less oxide inclusions in the steel,approximately over 16.7%MnS precipitates were with aspect ratio a>5 and pure MnS precipitates accounted for 75.9%in number.However,with more oxide inclusions in the steel,only 7.4%MnS precipitates were with a>5 and pure MnS precipitates accounted for 60.1%in number.Refinement of MnS by oxide inclusions improved the strength and inhibited the anisotropy.More oxide inclusions in the steel increased the yield strength and tensile strength of the steel in both longitudinal and transverse directions,and lowered the anisotropy of the mechanical property.

Distribution of oxide inclusions in H13 castings under super-gravity field with multi-stage rotation speeds

The 42 kg industrial H13 castings were prepared by different super-gravity fields with multi-rotation speeds,and the distribution of oxide inclusions in the castings was studied.In addition,the inward movement Reynolds number and inward movement time of oxide inclusions as well as the solidification time of molten steel at different positions in the castings were calculated to clarify the removal mechanism of oxide inclusions in super-gravity field.The results show that the large size(i.e.,greater than 10μm)oxide inclusions are mainly concentrated in the inner and outer parts of the super-gravity castings with constant rotation speed(500 r min^(-1))and five-stage rotation speeds(500,600,750,850,and 950 r min^(-1)),respectively,while there are no large oxide inclusions in the super-gravity castings with three-stage rotation speeds(500,600,and 750 r min^(-1)).Although an increase in the particle size of inclusion and the rotation speed in super-gravity field is conducive to the increase in the inward movement Reynolds number of oxide inclusions and reduction in the inward movement time of oxide inclusions,it will reduce the local solidification time of molten steel.In the range of the rotation speed studied,the super-gravity field with three-stage rotation speeds has the best effect on the removal of inclusions in H13 molten steel.

Effect of low basicity refining slag on evolution and removal of oxide inclusions in 55SiCrA spring steel

The laboratory experiments,thermodynamic analysis,dynamic analysis,and industrial trials were carried out to investigate the influence of refining slag on the evolution and removal of oxide inclusions in 55SiCrA spring steel.The reduction in basicity and Al_(2)O_(3) content in refining slag can reduce the[Al]s content in the molten steel,which is conducive to the control of the low melting point of inclusions.However,the refining slag with excessively low basicity transfers the oxygen element to molten steel and increases the Al_(2)O_(3) content in inclusions,which is harmful to the control of inclusions.According to the chemical compositions of inclusions and refining slag in laboratory experiments,their physical parameters were calculated.The maximum separation ratio and the moving time of inclusions to reach the maximum separation ratio(t_(max))of inclusions under different laboratory experimental conditions were studied.The maximum separation ratio of inclusions is positively correlated with the overall wettability(coshIMS)among the slag,steel,and inclusions.The maximum separation ratio of inclusions obtained by laboratory experiments is between 85%and 91%.The t_(max) decreases with the decline in basicity and Al_(2)O_(3) content of refining slag,but excessively low basicity will increase the t_(max).The basicity of refining slag in the range of 0.88–0.97 and the content of Al_(2)O_(3) less than 6%is not only conducive to reducing the content of Al_(2)O_(3) and the melting point of inclusions but also beneficial to removing the inclusions to the slag.The slag system shows good metallurgical results in industrial trials.

STUDY ON FORMATION MECHANISM OF ADHERING LAYER FORMED ON TOOL FACE

The appearance of adhenng layer formed on tool face, its composition and distributionare analysed when Ca-S free-cutting stainless steel is machined. Cutting temperature field and itsrelation with formation of the layer is also studied. The result shows that, the layer can be formed under proper temperature condition, the stable cutting temperature field keeps the stable layer, itsthickness and composition distribution along rake face depend on the corresponding cutting tem-perature field. The theoretical model of the layer formation is set up.

Effect of Calcium Treatment on Non-Metallic Inclusions in Ultra-Low Oxygen Steel Refined by High Basicity High Al_2O_3 Slag

The influence of calcium treatment on non-metallic inclusions had been studied when control technology of refining top slag in ladle furnace was used in ultra-low oxygen steelmaking. A sufficient amount aluminium was added to experimental heats for final deoxidizing during BOF tapping, and the refining top slag with strong reducibility, high basicity and high Al2O3 in ladle furnace was used to produce ultra-low oxygen steel and the transformation of nonmetallic inclusions in molten steel was compared by calcium treatment and no calcium treatment. The results show that the transformation of Al2O3--MgO - Al2O3 spinel-CaO-MgO-Al2O3 complex inclusions has been completed for aluminum deoxidation products and calcium treatment to molten steel is unnecessary when using the control technology of ladle furnace refining top slag to produce ultra-low oxygen steel, and the complex inclusions are liquid at the temperature of steelmaking and easily removable to obtain very high cleanliness steel by flotation. Further- more, the problems of nozzle clogging in casting operations do not happen and the remaining oxide inclusions in steel are the relatively lower melting point complex inclusions.

Characterization of the globular oxide inclusion ratings in steel using laser-induced breakdown spectroscopy

Grade assessment of steel is generally performed via the metallographic method, which is time-consuming and is not able to provide the elemental distribution information. In this paper, we present a method to measure the globular oxide inclusion ratings in steel using laser-induced breakdown spectroscopy (LIBS). The measurement is performed in two basic steps: steel samples are polished using metallographic sand paper and the Al2O3 inclusion number and size distribution in a marked area are observed using scanning electron microscope/energy dispersive X-ray spectroscopy (SEM/EDS) for further LIBS scanning analysis. The threshold intensity that distinguishes soluble aluminum and insoluble aluminum inclusions is determined using LIBS combined with the SEM/EDS statistical data. Carbon steel (the sample number is S9256) and bearing steel (the sample number is GCr15) are analyzed in scanning mode, and the number of Al2O3 inclusions in different size ranges is obtained from the statistical information derived from the Al2O3 size calibration curve. According to heavy and thin series for globular oxide inclusions grade assessment, the method we propose is comparable to the traditional metallographic method in terms of accuracy; however, the process is simplified and the measurement speed is significantly improved.

Oxide Inclusions in Ferromanganese and Its Influence on the Quality of Clean Steels

Low and medium carbon ferromanganese produced by oxygen decarburization process and electric silicothermic process was briefly introduced, and the quality of products by these two processes was analyzed. Results showed that the total oxygen content in medium carbon ferromanganese by electric silicothermic process in China, which ranged from 0.039% to 0.171%, was between those of the common and refined products by oxygen decarburization process outside of China. The increments of total oxygen content in liquid steel were estimated when ferromanganese was added for the purpose of Mn element adjustment at the end of smelting. Refined low and medium carbon ferromanganese, which had low total oxygen content, was recommended for composition adjustment of clean steels during final stage of a heat. It is possible that the inclusions in the ferromanganese alloy greatly influenced the quality of clean steel indirectly by affecting the amount, size and composition of inclusions in steel.

Additive manufacturing of a Co-Cr-W alloy by selective laser melting:In-situ oxidation,precipitation and the corresponding strengthening effects

Additive manufacturing exhibits great potentials for the fabrication of novel materials due to its unique non-equilibrium solidification and heating process.In this work,a novel nano-oxides dispersion strengthened Co28 Cr9 W1.5 Si(wt.%)alloy,fabricated by laser powder bed fusion(LPBF),was comprehensively investigated.During the layer-by-layer featured process,in-situ formation of Si rich,amorphous,nano-oxide inclusions was observed,whose formation is ascribed to the high affinity of Si to oxygen.Meanwhile,distinctive body-centered cubic(BCC)Co5 Cr3 Si2 nano-precipitates with an 8-fold symmetry were also confirmed to appear.The precipitates,rarely reported in previous studied Co-Cr alloys,were found to tightly bond with the in-situ oxidization.Furthermore,the morphologies,the size distributions as well as the microstructure of the interface between the matrix and the inclusions were investigated in detail and their influence on the tensile deformation was also clarified.The existence of transition boundaries between these inclusions and the matrix strongly blocked the movement of dislocations,thereby increasing the strength of the alloy.It was understood that when the plastic deformation proceeds,the fracture occurs in the vicinity of the oxide inclusions where dislocations accumulate.A quantitative analysis of the strengthening mechanism was also established,in which an additional important contribution to strength(~169 MPa)caused by the effects of in-situ formed oxide inclusions was calculated.

Effect of vanadium on modification of inclusions in Mn-and Si-deoxidized steel during heat treatment at 1 473 K

The effect of vanadium （V） on the modification of oxide inclusions in steels with different concentra- tions of Mn, Si, and V was determined before and after heat treatment at 1473 K. Changes in the morphology, size, and composition of these inclusions were analyzed. Equilibrium relations between the inclusions and steels at 1873 K and 1473 K were calculated using available thermodynamic data to roughly approximate the stable oxide inclusions in the steels, The results revealed that the concentra- tions of V and Si in the steel are critical for controlling the modification of the inclusions during heat treatment at 1473 K. MnO-SiO2-type oxide inclusions gradually transformed into MnO-V2O3-type or Mn-SiO2- and MnO-V2 O3-type inclusions in low Si high-V steels heat-treated for 60 min, In addi- tion, the morphology of the inclusions changed from spherical to irregular. A Si-accumulated zone and a V-depleted zone formed close to the interface in the steel matrix. The experimental and calcula- tion results indicated that, during the heat treatment, an interface chemical reaction occurred be- tween the Fe-Mn-Si-V steel and the MnO-SiO2 type oxide inclusion.

Interfacial reaction between oxide inclusion and steel matrix deoxidized by Si and Mn at 1473 K

An improved diffusion couple method was used to simulate the dynamic process of the solid-state reaction at the interface between oxide inclusions and a steel matrix deoxidized by Si and Mn during heat treatment at 1473 K. Experimental results indicated that good contact between the oxide and steel matrix was attained after pre-treatment at 1673 K. In addition, the reaction between the oxide and steel matrix at 1673 K was suppressed, and the effect of this reaction on the diffusion couple experiments at 1473 K was minimized. In the diffusion couple experiments, the diffusion of oxygen from the oxide to the steel matrix resulted in the precipitation of fine oxide particles and a decrease in the Mn content in the steel matrix near the interface after heat treatment at 1473 K. With increasing heat treatment time, the widths of the particle precipitation zone （PPZ） and Mn-depleted zone （MDZ） gradually increased. In addition, the solid-state reaction at the interface between the oxide and steel matrix was intense, and the widths of the PPZ and MDZ increased rapidly during the 0-20 h stage of heat treatment, especially during the 0-5 h stage. The interfacial reaction was retarded, and the rates of width expansion of PPZ and MDZ decreased with increasing heat treatment time.

In-situ observation of asymmetrical deformation around inclusion in a heterogeneous additively manufactured 316L stainless steel

Oxide inclusions widely exist in additively manufactured components due to the native oxide layer on the powder surface,together with gas impurities during the printing process.Using in-situ tensile tests combined with electron backscatter diffraction(EBSD)and electron channeling contrast imaging(ECCI)techniques,we propose an asymmetrical cracking mechanism around the oxide inclusions in a selective laser melted 316L stainless steel.The heterogeneous sub-micro cellular structures lead to different twinning tendencies around the inclusions due to the size-related critical twinning stresses,and the deformation-induced nano-twin clusters can resist the cracking propagation,therefore resulting in the asymmetrical cracking behaviors around the inclusions.

Cleanliness of Alloying Structural Steel

Alloying structural steel used for mechanical structures has a high requirement for cleanliness because its failures are greatly affected by non-metallic inclusions and total oxygen content in steel.It has been reported by some steelmaking plants to have some problems in controlling total oxygen content and inclusions during alloying structural steel production.For this purpose,cleanliness control in 0.2C-0.3Si-0.6Mn-1Cr-0.2Mo steel was investigated.Firstly,low melting temperature zone（≤1873 K） of CaO-Al2O3-MgO system and formation condition of low melting temperature inclusions were investigated through thermodynamic equilibrium calculation.On this basis,industrial tests were carried out.Through sampling at different stages,transformation of oxide inclusions and change of total oxygen content in steel were studied.The results show that：in order to form CaO-Al2O3-MgO system inclusions with low melting temperature,mass percent of Al2O3,MgO and CaO in inclusions should be controlled from 37.6% to 70.8%,0 to 17.4% and 25.5% to 60.6%;For the condition of 1873 K and 0.05%（mass percent） dissolved aluminum in steel,the activities of dissolved oxygen,magnesium and calcium should be controlled as 0.298×10-4-2×10-4,0.1×10-5-40×10-5 and 0.8×10-8-180×10-8 respectively.With secondary refining proceeding,average total oxygen content and inclusion amount decrease,the type of most inclusions changes from Al2O3 after tapping to Al2O3-MgO after top slag is formed during ladle furnace refining and finally to CaO-Al2O3-MgO after RH treatment.In the final products,average total oxygen content was 12.7×10-6 and most inclusions were in spherical shape with size less than 5 μm.

Helium Bubble Growth in He^(+) Ions Implanted 304L Stainless Steel Processed by Laser Powder Bed Fusion During Post-Irradiation Annealing at 600℃

The abundancy of defect sinks in the microstructure of laser powder bed fusion(LPBF) processed austenitic stainless steels was found to be beneficial for helium resistance.In the current study,the influence of the novel microstructure in LPBF processed 304 L on the helium bubble growth behaviour was investigated using transmission electron microscopy in samples implanted with He^(+) ion and post-irradiation annealing treated at 600℃ for 1 h.Two variants of LPBF processed 304 L samples were used,one in as-built condition and the other solution-annealed.The comparison between the two samples indicated that the helium bubble growth was inhibited and remained stable in the as-built sample but coarsened significantly in the solution-annealed sample.The sub-grain boundaries and oxide nano-inclusions acted as defect sinks to trap helium atoms and inhibited the growth of helium bubble in the as-built sample under the post-irradiation annealing conditions used.