High-temperature Laser Scanning Confocal Microscopy Research Articles

In-situ observation of solidification process in β-solidifying γ-TiAl-based alloy

The solidification process of Ti-40Al alloy, a representative β-solidifying γ-TiAl-based alloy, is investigated in-situ using high-temperature laser scanning confocal microscopy (HTLSCM). During the heating process, Ti-40Al alloy exhibits a complete β phase microstructure; however, peritectic α phase is observed during solidification. The occurrence of peritectic α phase is discussed and attributed to the segregation of Al under certain solidification conditions. This finding is further confirmed in the directional solidification of another β-solidifying γ-TiAl-based alloy, TNM alloy, and it provides valuable guidance for controlling the microstructure of β-solidifying γ-TiAl-based alloys.

Comparative study of the strain and strain rate hardening mechanisms and its workability during hot deformation of TC4 titanium alloys

Localized thinning is one of the main defects in hot forming processes, which is determined by the hardening behaviour during deformation. This study focused on building a hot-workability map to prevent localized thinning in wide ranges (650–950 °C & 0.001–1 s−1) for industrial significance. Insights into the associated strain and strain rate hardening mechanisms were provided by visualizing the microstructure evolutions using both in-situ High-Temperature Laser Scanning Confocal Microscope (HTLSCM) and Electron Backscattered Diffraction (EBSD). Results show that the highest uniform strain, up to 0.250, is achieved in the viscoplastic region due to the cooperative strain and strain rate hardening, where dislocation slip, α/β transformation and grain sliding concurrently occur. Significant grain refinement is also achieved. The optimum forming condition was identified in the viscoplastic region and is further verified by forming an ultra-thin large bend component, reducing thickness unevenness from 18.6 % to 13.1 %. This research finding could aid in understanding the effects of strain and strain rate hardening on forming uniformity and further provide scientific guidance for industrial processing parameters selection, reducing localized thinning and hence scrap rates.

In Situ Microstructural Evolution and Precipitate Analysis of High-Nickel Shipbuilding Steel Using High-Temperature Confocal Laser-Scanning Microscopy

This study investigates the microstructural evolution and mechanical properties of high-nickel shipbuilding steel during thermal processing using high-temperature confocal laser-scanning microscopy (HTCLSM). An in situ observation of the heating and holding processes reveals critical insights into phase transformations, grain-growth behavior, and the formation of precipitates. The experimental results demonstrate that austenitization begins at approximately 700 °C, with significant grain-boundary nucleation. At 900 °C, the formation of black precipitates was observed, and their persistence up to temperatures exceeding 1000 °C was confirmed. Scanning electron microscopy (SEM) and energy-dispersive spectroscopy (EDS) analyses identified these precipitates as chromium carbides (Cr7C3), which significantly contribute to the material’s strength. A comprehensive analysis using transmission electron microscopy (TEM) confirmed the presence and distribution of Cr7C3 within the grains and along grain boundaries. These findings provide a deeper understanding of the microstructural dynamics in high-nickel steels, guiding the optimization of heat-treatment processes to enhance mechanical properties for maritime applications.

Deep learning revealed statistics of the MgO particles dissolution rate in a CaO–Al2O3–SiO2–MgO slag

Accelerated material development for refractory ceramics triggers possibilities in context to enhanced energy efficiency for industrial processes. Here, the gathering of comprehensive material data is essential. High temperature-confocal laser scanning microscopy (HT-CLSM) displays a highly suitable in-situ method to study the underlying dissolution kinetics in the slag over time. A major drawback concerns the efficient and accurate processing of the collected image data. Here, we introduce an attention encoder–decoder convolutional neural network enabling the fully automated evaluation of the particle dissolution rate with a precision of 99.1%. The presented approach provides accurate and efficient analysis capabilities with high statistical gain and is highly resilient to image quality changes. The prediction model allows an automated diameter evaluation of the MgO particles' dissolution in the silicate slag for different temperature settings and various HT-CLSM data sets. Moreover, it is not limited to HT-CLSM image data and can be applied to various domains.

Effects of rare earth modifying inclusions on the nucleation mechanism and mechanical properties of MC5 roller steel

The effect of Ce treatment on the inclusions and mechanical properties of MC5 roller steel after solidification and annealing process was investigated. The implementation was observed by thermodynamic calculation, Electron Probe Micro-Analyzer and high-temperature confocal laser scanning microscopy (HT-CLSM). The results showed that as rare earth content increase, the inclusions were effectively modified into cerium oxide (Ce-O) and cerium sulfide (Ce-O-S); Compared with 0 RE steel, eliminating the proportion of inclusions larger than 5 μm by 14% and 22%; the average size decreased to 3.60 μm and 2.30 μm. Subsequently. CLSM was used to observe the aggregation, separation and agglomeration behavior of MgAlO4 inclusions and alloy elements on the surface of molten steel. Moreover. the ultimate tensile strength and yield strength of MC5 roller steel with Ce treatment increased by 12.6% and 34%. The addition of rare earths could improve the of MC5 roller steel, it provides effective reference value for subsequent industrial experiments.

Versatile fluidity test model for cast superalloys and comparison between IN718 and IN939

A spiral fluidity test model of superalloys with 10 mm in height and 3 mm in thickness was designed to evaluate the fluidity of two distinct Ni-based superalloys IN718 and IN939. The factors influencing fluidity are ascertained through comparative analysis utilizing methodologies such as JMatPro, differential scanning calorimetry and high-temperature confocal laser scanning microscopy. The results show that under identical testing conditions, the fluidity of the IN939 superalloy surpasses that of the IN718 superalloy. When subjected to the same temperature, the melt viscosity and surface tension of IN939 superalloy are considerably reduced relative to those of IN718 superalloy, which is beneficial to improving the melt fluidity. Furthermore, the liquidus temperature and solidification range for the IN939 superalloy are both smaller compared with those of the IN718 superalloy. This condition proves advantageous in delaying dendrite coherency, thereby improving fluidity.

Formation mechanism of cracks formed during drilling of a cold drawn prestressing 1215 free-cutting steel

1215 steel is a low-carbon free-cutting steel with the largest production, and its quality issues are complex and diverse. The formation mechanism of cracks formed during drilling of a cold drawn prestressing 1215 free-cutting steel was investigated by means of optical microscopy, scanning electron microscopy, high-temperature laser scanning confocal microscopy, and Thermo-Calc software. The failure was caused by abnormally wide pearlite with large amounts of sulfide nearby. We speculate the abnormal microstructure was related to C and S segregation in columnar-to-equiaxed transition zone during continuous casting process. However, element segregation was an inherent property in the continuous casting process. Reheating was an important process for homogenization to eliminate segregation, but the reheating temperature was lowered to reduce production costs. The lower reheating temperature resulted in incomplete elimination of columnar-to-equiaxed transition zone segregation, ultimately leading to the formation of abnormal microstructure. This batch of 1215 steel wire was not suitable for producing component required transverse plasticity during machining, but could be used to produce circular shaft components. In the future, it is suggested to increase the reheating and hot-rolling temperature, or take effective measures to reduce segregation during continuous casting.

Solidification and microstructure investigation on as-cast and annealed hypoeutectic Ti–Fe alloys

This work explored the solidification behavior, microstructure development, and resulting mechanical properties of hypoeutectic Ti–Fe alloys under both as-cast and annealed conditions. Ti-(27, 28, 29)Fe (wt%) alloys were synthesized through arc-melting, followed by annealing at 950 °C for 24 h and slow furnace cooling. The investigation procedures included thermodynamic calculations, differential scanning calorimetry, scanning electron microscopy, high-temperature laser-scanning confocal microscopy, X-ray diffraction, hardness measurements, and compression tests. The study demonstrated the efficacy of annealing treatments in reducing excess eutectic in the as-cast structure formed during solidification. Results from both thermodynamic calculation and experiment for the solidification process demonstrated reasonable agreement. The high β-stabilizing effect of Fe ensured the presence of the β phase at room temperature under both studied conditions. The solid-solution hardening of the β phase, coupled with the TiFe intermetallic, substantially contributed to the increased hardness and mechanical strength, although the increase in brittleness was noticeable in the as-cast state. Subsequent annealing enhanced plasticity but resulted in a reduction in strength, albeit maintaining yield strength at a considerable level, approximately 1450 MPa.

Influence of Solute Drag Effect and Interphase Precipitation of Nb on Ferrite Transformation.

The significant impact of Nb on ferrite transformation, both in terms of solute drag effect (SDE) and interphase precipitation, was investigated quantitatively. Ferrite transformation kinetics were characterized using thermal expansion experiments and theoretical calculations. The microstructures were characterized using high-temperature confocal laser scanning microscopy (CLSM), a field-emission scanning electron microscope (FESEM), and a transmission electron microscope (TEM). Under a higher driving force, interphase precipitations were observed in the sample with a higher Nb content. A three-dimensional (3D) reconstruction method was used to convert the two-dimensional (2D) image of interphase precipitation into a three-dimensional model for a more typical view. The SDE and interphase precipitation had opposite effects on the kinetics of ferrite transformation. A lower Nb content showed a strong contribution to the SDE, which delayed ferrite transformation. A higher concentration of Nb was expected to enhance the SDE, but the inhibition effect was eliminated by the interphase precipitation of NbC during interfacial migration. Both the experimental results and theoretical calculations confirmed this phenomenon.

Improvement in Grain Size Distribution Uniformity for Nuclear-Grade Austenitic Stainless Steel through Thermomechanical Treatment.

In this work, thermomechanical treatment (single-pass rolling at 800 °C and solution treatment) was applied to nuclear-grade hot-rolled austenitic stainless steel to eliminate the mixed grain induced by the uneven hot-rolled microstructure. By employing high-temperature laser scanning confocal microscopy, microstructure evolution during solution treatment was observed in situ, and the effect of single-pass rolling reduction on it was investigated. In uneven hot-rolled microstructure, the millimeter-grade elongated grains (MEGs) possessed an extremely large size and a high Schmid factor for slip compared to the fine grains, which led to greater plastic deformation and increased dislocation density and deformation energy storage during single-pass rolling. During subsequent solution treatment, there were fewer nucleation sites for the new grain, and the grain boundary (GB) was the main nucleation site in MEGs at a lower rolling reduction. In contrast, at a higher reduction, increased uniformly distributed rolling deformation and more nucleation sites were developed in MEGs. As the reduction increased, the number of in-grain nucleation sites gradually exceeded that of GB nucleation sites, and in-grain nucleation preferentially occurred. This was beneficial for promoting the refinement of new recrystallized grains and a reduction in the size difference of new grains during recrystallization. The single-pass rolling reduction of 15-20% can effectively increase the nucleation sites and improve the uniformity of rolling deformation distribution in the MEGs, promote in-grain nucleation, and finally refine the abnormally coarse elongated grain, and eliminate the mixed-grain structure after solution treatment.

Mechanistic insight into phosphorus migration pathways from oolitic hematite using in-situ observations during roasting and reduction process

Oolitic hematite is a promising alternative resource, in facing the iron ore downgrading. As oolitic hematite is often rich in phosphorus, an efficient separation of iron and phosphorus is necessary, in terms of utilizing both elements. Therefore, a close insight into the transformation of phosphorus-bearing minerals in the unique oolitic structure during the reduction process is important. To capture the real-time transformation of the apatite ring in the oolitic structure, in-situ observations under roasting, and CO/carbon reducing conditions were adopted by high-temperature confocal laser scanning microscopy. The results indicated that the apatite ring was transformed by four stages during the roasting process from 25 °C to 1400 °C: stabilization, defluorination, partial melting, and complete melting, which was: Ca5(PO4)3F → Ca3(PO4)2 → Ca3(PO4)2 + P2O5 liquid → P2O5 liquid. Under the CO reduction, the partial reduction of the phosphate at 1400 °C generated a Fe-Plow alloy. While the carbon reduction promoted iron phase absorption of phosphorus, forming Fe-Phigh alloy at 1400 °C. In addition, interfacial phenomena between apatite and slag melt were observed, and the dissolution of apatite (Ca/P molar ratio) into the slag melt was affected by the Fe/(Al + Si) molar ratio of the slag. Finally, using inverse error function methods, the diffusion coefficients of P and Ca increased significantly from the roasting to CO reduction and then to carbon reduction. These findings can benefit to understand phosphorus migration mechanisms, improving effective dephosphorization strategies for high-phosphorus oolitic hematite.

In-situ observation of restoration of tungsten plate via high-temperature confocal laser scanning microscopy

The restoration of an yttria dispersion strengthened tungsten plate and the corresponding microstructural evolution are investigated through in situ annealing using high-temperature confocal laser scanning microscopy. The geometrically necessary dislocation density and subgrain/grain evolution at each annealing stage are confirmed using the electron backscatter diffraction technique. The microstructure's evolution is divided into distinct stages of recovery, recrystallization, and grain growth based on their characteristic features. During the recovery process, the fomation of subgrains occurs. The primary mechanism of recrystallization nucleation is dominated by the strain-induced boundary migration mechanism, and the subgrains preexisting at grain boundaries are the main nucleation sites.

Physicochemical transformation of gasification slags with different residue carbon contents during sintering/melting process

The ash residue after gasification in the coal gasifier contains a certain proportion of residual carbon, which exerts a significant effect on the slag properties such as sintering, melting, and flow within the furnace. The residues discharged outside the gasifier retain the distribution patterns of ash and residual carbon under gasification conditions. This study selected coarse and fine residues generated from an entrained-flow gasifier and investigated the transformation of slags with different carbon contents during heating process. The obtained ash residues underwent characterization to determine the modes of the compositions occurrence. Subsequently, ash residues with different carbon contents were observed for the sintering-melting processes with a high-temperature confocal scanning laser microscope (CSLM). With the aid of FactSage, the physicochemical transformation of slag particles was determined. The impact of residual carbon on particle characteristics manifests in both physical structure and chemical reactions. On one hand, residue residual carbon can act as a skeleton during the melting process, causing the molten phase to enter the pores of porous carbon, intensifying particle shrinkage. After the inorganic components melt, the liquid encapsulated by carbon retains the original particle shape. On the other hand, the carbon can react with the inorganic ash components. If the carbon content is less than 6%, a new FexSi with a high ash melting point can be formed. As the carbon content increases, the carbon reacts with the Si to form SiC. This implies a reduction in the liquid content. Therefore, the flow temperature is greatly delayed by an increase in carbon content above 14%.

Effect Mechanism of α-Ferrite Sustained Precipitation on High-Temperature Properties in Continuous Casting for Peritectic Steel

Exploring the mechanism of the α-ferrite precipitation process on high-temperature properties plays an important guiding role in avoiding slab cracks and effectively regulating quality. In this work, in situ observation of the α-ferrite sustained precipitation behavior for peritectic steel during the austenitic phase transition process has been investigated using high-temperature confocal scanning laser microscopy. Meanwhile, the high-temperature evolution of the phase fractions during the phase transition process was quantitatively analyzed based on the high-temperature expansion experiment using the peak separation method. Furthermore, the high-temperature properties variations of the casting slab during the α-ferrite sustained precipitation process were investigated with the Gleeble thermomechanical simulator. The results show that the film-like ferrite precipitated along the austenite grain boundaries at the initial stage of phase transition, then needle-like ferrite initiates rapid precipitation on film-like ferrite when the average thickness reaches 15~20 μm. Hot ductility reached a minimum at the ferrite phase fraction fα = 10~15%, while high-temperature properties returned to a higher level after fα > 40~45%. The appearance of a considerable amount of needle-like ferrite and grain refinement effectively improves the high-temperature properties with the α-ferrite precipitation process advances.

In situ study and assessment of the phosphorus-induced solute drag effect on the grain boundary mobility of austenite

The solute drag effect of phosphorus (P) in the single-phase austenite (γ-Fe) region was studied under isothermal annealing conditions at temperatures of 1050 °C, 1150 °C, 1250 °C and 1350 °C. High-temperature laser scanning confocal microscopy (HT-LSCM) was used to observe and quantify in situ grain growth on the surface of three different samples containing 0.026 wt.-% P, 0.044 wt.-% P and 0.102 wt.-% P. The dependence of the arithmetic mean grain sizes on time and temperature were modeled mathematically using a simple ordinary differential equation (ODE) according to normal grain growth (NGG) theory. As no other major effects, i.e., Zener-pinning by precipitates, occurred under the selected experimental conditions, grain growth interference was only considered by grain boundary (GB) segregation of P. Thus, the total grain boundary mobility (M) was directly determined depending on the P content and isothermal annealing temperature. The fitted GB mobility values enabled the determination of an average binding energy value between impurity P atoms and grain boundaries (E0 = -1.1 - -0.6 eV) in the system. Finally, the GB segregation of P in γ-Fe was derived from the observed grain growth kinetics. The results showed reasonable agreement with calculations using segregation enthalpies from the literature.

Detachment of a Soluble Particle at the Slag-Argon Interface: CFD Study and Experimental Observations

The behavior of non-metallic inclusions at interfaces of high-temperature melt and molten slag affects the removal of inclusions and the consequent melt cleanness. This study presents real-time in situ observations on the behavior of an oxide particle in the vicinity of the slag-argon interface by means of high-temperature confocal scanning laser microscopy (HT-CSLM). On top of that, CFD simulations are conducted to investigate the underlying mechanisms of particle-interface interactions. In addition to revealing the particle motion process from the argon phase toward the slag, a significant particle morphology alteration associated with its dissolution in the slag is experimentally observed. Particularly, upon detachment from the slag-argon interface, the particle exhibits more dissolution at the near-interface area. By combining with numerical simulations, this study indicates that particle separation at the interface can be characterized as two stages. First, a short-term capillary force-driven motion stage happens until the particle initially settles at the interface. The settling position estimated by simulation shows good consistency with experimental measurement. Second, the particle takes a relatively long time to eventually detach from the interface, and this period is accompanied by particle dissolution. Investigations suggest that the concentration variation near the interface arising from particle dissolution triggers a Marangoni flow. This flow, in turn, enhances the local dissolution rate, consequently causing a significant particle morphology change that influences the detachment. This study provides new insight into the mechanism of inclusion removal through slag absorption in metallurgical processes. Both particle dynamics and dissolution kinetics, especially the effect of solutal Marangoni convection, are highlighted in detaching a small-scale particle from the fluid-fluid interface.

Inclusions and microstructures in coarse-grained heat-affected zone of Al–Ti–Ca deoxidized shipbuilding steels with different Al contents after high-heat input welding

The inclusions, microstructure evolution and impact toughness of the coarse-grained heat-affected zone (CGHAZ) of Al–Ti–Ca deoxidized shipbuilding steel plates with different Al contents after high-heat input welding of 400 kJ cm−1 are investigated. The characteristics of inclusions and their influence on the refinement of microstructure and impact toughness in CGHAZ was elucidated. Increasing the Al content from 0.016 wt% to 0.022 wt% and 0.043 wt% results in an increase in the average size of prior austenite grain and the brittle phase fractions, while decreasing the content of intragranular acicular ferrites (IAFs). The results of the thermodynamic calculations, high-temperature laser scanning confocal microscopy and differential scanning calorimetry all show that increasing the Al content can diminish the austenitic stable region, elevate the transition temperature from austenite to ferrite and suppress the nucleation of IAF. In the present steels, the IAF formation is successfully induced by the specific inclusions, namely Al2O3–CaO–Ti2O3–MnS(-CaS), in which the calcium aluminate inclusions are embedded with Ti-oxides and CaS–MnS precipitates. The effective inclusions have the number density of 93 mm−2 in 16Al steel and 27 mm−2 in 22Al steel, but they are rarely found in 43Al steel. On average, an effective inclusion can induce 3.4 IAFs in 16Al steel and 2.8 IAFs in 22Al steel. Thus, as the Al content increases from 0.016 wt% to 0.22 wt% and 0.043 wt%, the impact toughness of CGHAZ at −40 °C decreases from 134 J to 78 J and 24 J with the welding heat input of 400 kJ cm−1.

In-situ observation of Ni-11.5 wt%Si eutectic microstructure evolution and exploration of strengthening mode of Ni-Ni3Si eutectic composites

Microstructure evolution of the Ni-11.5 wt%Si eutectic alloy during the melting and cooling process was elaborately examined using a high-temperature confocal laser scanning microscope (HT-CLSM). The thermal stability of the phase composition within the Ni-11.5 wt%Si eutectic alloy was thoroughly analyzed. The intricate mechanism governing the solidification of the Ni-11.5 wt%Si eutectic alloy, along with the formation of the metastable Ni31Si12 phase under varying cooling rates, was systematically investigated. Through in-depth in-situ observations, a well-defined heat treatment procedure was developed for Ni-Ni3Si eutectic composites. Remarkably, the metastable Ni31Si12 phase can completely transform into Ni3Si upon undergoing the prescribed heat treatment, yielding a refined lamellar structure. This structural refinement notably results in substantial enhancements in the compressive properties and fracture toughness of the Ni-Ni3Si eutectic composite at ambient temperatures.

Phase-field simulation and high-temperature confocal laser scanning microscope experimental study of Martensite transformation during the disk laser quenching process

Laser quenching has significant advantages over conventional heat treatment. The main microstructure of C30E4 steel after quenching at a specific temperature is Martensite. Accurately obtaining the microscopic characteristics of the Martensite transformation process is the key to obtaining the best material properties, which is significant to material design. In this paper, the C30E4 steel was disk-laser-quenched, the metallographic and high-temperature confocal laser scanning microscope experiment was carried out. The microstructure of the fully phase-change hardened zone, heat-affected transition zone and matrix zone after quenching was obtained. The C30E4 martensitic transformation process in-situ was obtained. The mathematical physics model of Martensite transformation from metastable to steady state was established by phase field method. The finite-element method was used to solve the model, and the quenching Martensite transformation law was obtained. The Martensite formation process in austenite grain boundaries and microstructure defects was discussed. The experimental and the numerical simulation were compared to get consistent results, which verify the validity of the calculation method. This study lays a significant foundation for effectively revealing the Martensite formation and transformation during the disk laser quenching process, and provides a theoretical basis for quantifying the influence of Martensite transformation process on material properties.

Formation and modulation mechanisms of Fe-As phases in melting-processed Ba(Fe1-xCox)2As2 superconductor

The Fe-As phases play a crucial role in determining the superconducting properties of iron arsenic-based superconductors. In this study, we employed high-temperature confocal laser scanning microscopy (HT-CLSM) to investigate the formation mechanism of Fe-As phases in the melting processed Ba(Fe0.92Co0.08)2As2 superconductor through in situ observations. By combining these observations with microstructural and magnetic characterizations, we have confirmed that the high-temperature Fe-As phases primarily originate from the partial incongruent melting of the Ba122 superconducting phase. Moreover, we have elucidated the transition process of the Fe-As liquid and identified two dominant eutectic reactions in normal cooling sample: "L → Fe2As + FeAs" and "L → Fe2As + α-Fe". In case of extremely slow cooling rate, a further eutectic reaction between the Fe-As and superconducting phases ("L → Ba122 + Fe2As + FeAs") occurs, leading to the elimination of α-Fe and an increased volume of non-superconducting phases. We have also analyzed the effects of the Fe-As phases on the magnetic behavior, critical current density, and vortex pinning behavior. This study provides valuable insights for designing the microstructure of new type iron arsenic-based superconductors through the melting process.