High-temperature Laser Scanning Confocal Microscopy Research Articles

Evolution of primary carbides during accelerated solidification process of high-carbon martensitic stainless steels

In order to evaluate the potential application advantage for development of sub-rapid cooling strip casting of high-carbon martensitic stainless steels, the effects of cooling rate on the solidification microstructure, solute element segregation, and primary carbide precipitation in high-carbon martensitic stainless steels were investigated using an association of high-temperature confocal laser scanning microscopy (HT-CLSM), optical microscopy (OM), scanning electron microscopy (SEM) and electro-probe microanalysis (EPMA). As a result, the microstructure becomes more refined and the secondary dendrite arm spacing (SDAS) decreases greatly by 51 μm from 65.9 μm as the increase of cooling rate from 30 to 6000 °C·min−1. The equation of SDAS versus cooling rate was formulated as λ2 = 191.62·RC−0.317. Solute elements are enriched in the inter-dendritic region, leading to the precipitation of primary carbides. The elemental segregation ratio reduces by more than 20 % for all elements, meanwhile, the size of primary carbides decreases significantly and the mean area fraction of the primary carbides decreases from 4.77 % to 0.82 % with increase of cooling rate from 30 to 6000 °C·min−1. Moreover, the reticulated carbides gradually become less continuous. Despite the type of carbide is not sensitive to the cooling rate, the content of Cr and Fe in the primary carbide is sensitive to cooling rate. Compared to the reported methods, sub-rapid cooling of strip casting shows great advantage in control of primary carbides of high-carbon martensitic stainless steels.

In Situ Observation the Effect of Y on the Solidification Process of 7Mo-SASS under a Low Cooling Rate.

The effects of Y on the solidification process of 7Mo super austenitic stainless steel (7MoSASS) under low cooling rate conditions (10 °C/min) were investigated using high-temperature confocal laser scanning microscopy (HT-CLSM). The in situ observation results indicate that Y samples promote an increase in austenite nucleation density. After 10 s of nucleation, the nucleation density increased by 149.53/mm2 for the Y sample. Furthermore, variance analysis indicated that Y addition improved the uniformity of the 7MoSASS solidification microstructure under low cooling rate conditions. The Johnson-Mehl-Avrami-Kolmogorov (JMAK) theory results showed that when the solid phase ratio was 0.5, the nucleation mode of the Y sample transitioned from saturation site nucleation to saturation site nucleation + Avrami nucleation. YAlO3 has a low lattice disregistry value with austenite, making it a suitable heterogeneous nucleation core for promoting the early nucleation of austenite. During the late stages of solidification, Y accumulates in the residual liquid phase, providing a greater degree of compositional undercooling. SEM-EDS analysis showed that Y contributed to the refinement of the 7MoSASS solidification microstructure, with the proportion of precipitated phases decreasing by approximately 7.5%. Cr and Mo were the main elements exhibiting positive segregation in 7MoSASS, and the Cr segregation ratio increased in the Y sample, while the Mo segregation ratio decreased.

Research on hot isostatic pressing sintering behavior of 90W–Ni–Fe–Cu alloy

In order to understand the underlying material evolution during liquid phase sintering (LPS) process in hot isostatic pressing process (HIP), microstructure and mechanical properties of 90 W–Ni–Fe–Cu alloys fabricated at 1400 °C/150 MPa are examined systematically. For 90W-4.2Ni-1.8Fe–4Cu alloy, the typical LPS microstructure, which are spherical W grains uniformly surrounded by continuously distributed γ- (Ni, Fe, Cu) matrix phase with the lowest W–W contiguity of 0.31, is achieved successfully after HIP at 1400 °C/150 MPa. The excellent tensile strength reaches as high as 873 MPa with elongation of 17.3% due to the soft γ- (Ni, Fe, Cu) matrix phase. Moreover, the relationship between the microstructure parameters VM(1−CW−W) and elongation ε are established and analyze the association with dislocation motion in depth through electron backscattered diffraction (EBSD) characterization. To our best knowledge, the LPS behavior of tungsten alloy is in-situ revealed by high-temperature confocal scanning laser microscopy (HT-CSLM) for the first time. The current research provides a novel strategy for designing and fabricating powder metallurgy materials by LPS with pressure.

Combination of In Situ Confocal Microscopy and Calorimetry to Investigate Solidification of Super‐ and Hyper‐Duplex Stainless Steels

The solidification processes of super‐ and hyper‐duplex stainless steels (i.e., UNS S32750 and S 33 207) are investigated in situ by a high‐temperature confocal laser scanning microscope (HT‐CLSM) and differential scanning calorimetry (DSC). The variations of δ‐ferrite phase fraction during solidification are measured quantitatively. The results show that liquid L→δ‐ferrite transformation first occurs at a certain degree of supercooling during the solidification process of steel. UNS S3DSS 3207 with a higher Cr content can result in a higher nucleation temperature and faster growth of δ‐ferrite compared to those of UNS S332750 steel. Moreover, both the liquidus (TL) and solidus temperatures (TS) are increased with the increasing Cr content, while TL increases greater than TS. Electron microscopies are used to quantify the fraction and composition of each phase. Scheil equation is employed to predict the distribution behavior of the main alloying elements in the solidification process, and the predicted results are consistent with the experimental findings. This study aims to provide real‐time experimental insights into the solidification kinetics of state‐of‐the‐art high‐alloy‐grade duplex steels and benefits for controlling the casting process in the real production of stainless steels.

Dissolution of Magnesia in Silicate Melts and Diffusivity Determination from CLSM Studies

Magnesia is one of the vital and extensively used refractory components. In this study, the dissolution of magnesia is investigated at 1450, 1500, and 1550 °C in three silicate slags in the CaO–Al2O3–SiO2–MgO system using high-temperature confocal laser scanning microscopy to determine its effective binary diffusivity. The pore-free fragments of single-crystal fused magnesia particles were used, and the effects of experimental parameters and slag properties on the dissolution of magnesia were assessed. The ranking of dissolution times in the three slags at the three temperatures did not agree with the trend expected from the CaO/SiO2 ratio of each slag. Instead, several quotients serving as reference numbers were tested. The effective binary diffusivities were calculated considering all the impacting phenomena and parameters. The diffusivities of magnesia at 1500 °C in the slags with CaO/SiO2 weight ratios of 0.65, 0.93, and 1.17 are 2.67 × 10−10, 1.81 × 10−10, and 3.20 × 10−10 m2/s, respectively. The diffusivity of magnesia in one of the three slags was compared with rotating finger test results, which showed good agreement. The plausibility of diffusivity was checked using an Arrhenius plot.

Effect of Cooling Rate on Crystallization Behavior during Solidification of Hyper Duplex Stainless Steel S33207: An In Situ Confocal Microscopy Study

Hyper duplex stainless steel (HDSS) is a new alloy group of duplex stainless steels with the excellent corrosion resistance and mechanical properties among the existing modern stainless steels. Due to the incorporation of the high content of alloying elements, e.g., Cr, Ni, Mo, etc., the crystallization behavior of δ-ferrite from liquid is of vital importance to be controlled. In this work, the effect of the cooling rate (i.e., 4 °C/min and 150 °C/min) on the nucleation and growth behavior of δ-ferrite in S33207 during the solidification was investigated using a high-temperature confocal scanning laser microscope (HT-CLSM) in combination with electron microscopies and thermodynamic calculations. The obtained results showed that the solidification mode of S33207 steel was a ferrite–austenite type (FA mode). L→δ-ferrite transformation occurred at a certain degree of undercooling, and merging occurred during the growth of the δ-ferrite phase dendrites. Similar microstructure characteristics were observed after solidification under two different cooling rates. The variation in the area fraction of δ-ferrite with different temperatures and time intervals during the solidification of S33207 steels was calculated at different cooling rates. The post-microstructure as well as its composition evolution were also briefly investigated. This work shed light on the real-time insights for the crystallization behavior of hyper duplex stainless steels during their solidification process.

Precipitation mechanism of σ phase in S32654 super austenitic stainless steel

By utilizing High-Temperature Confocal Laser Scanning Microscopy (HT-CLSM), the microstructure evolution of S32654 super austenitic stainless steel was observed in situ during both solidification and solid-state phase transition. Moreover, the predominant focus was on investigating the precipitation mechanism of the σ phase. The findings revealed that the initial stages of the solidification process involved the nucleation and growth of austenite, followed by a gradual reduction in the residual liquid phase between dendrites until complete solidification was achieved. Furthermore, as the temperature decreased, the composition of the austenite formed from the residual liquid phase differed from the initially formed austenite, ultimately leading to the formation of granular austenite through extrusion. Below the critical temperature, the excessive amounts of Cr and Mo could not be dissolved in the supersaturated austenite between dendrites, thereby resulting in the instantaneous eutectoid decomposition of austenite, namely γ → γ2 + σ.

The Role of MX Carbonitrides for the Particle-Stimulated Nucleation of Ferrite in Microalloyed Steel

The role of titanium and vanadium carbonitrides (Ti,V)(C,N) of the MX series on the austenite-to-ferrite transformation in microalloyed steels and their potential of acting as pre-nuclei for intragranular ferrite nucleation is examined experimentally and by computational simulation. Thermal treatments and single-hit compression tests are performed on a dilatometer and a Gleeble® 3800 thermomechanical simulator to investigate the phase transition and precipitation sequences within microalloyed steel. The analysis of the microstructure and examination of formed precipitates is carried out by using scanning electron microscopy (SEM) and transmission electron microscopy (TEM). In situ observations are realized via high-temperature laser scanning confocal microscopy (HT-LSCM). The experimental results are compared to kinetic precipitation simulations for MX precipitates’ particle-stimulated intragranular ferrite formation using an on-particle nucleation model for ferrite on the surface of the MX carbonitrides. A particular focus is the comparison of precipitation trends between non-deformed and deformed samples. The physically appropriate modeling of MX precipitation kinetics in combination with intragranular ferrite formation serves as a basis for future industrial process optimizations without extensive experimental work.

High-temperature rheological behavior and non-isothermal pyrolysis mechanism of macerals separated from different coals

It is a challenge to accurately characterize the caking behavior of coal after thermal softening and its reaction mechanism. In this work, the formation behavior of metaplast during coal macerals coking was investigated using high-temperature confocal laser scanning microscopy and high-temperature small-amplitude oscillatory shear rheometer, the source of diversities in thermal fluidity of coal was revealed by thermogravimetric-mass spectrometry analysis and kinetic-thermodynamic theory calculations. The results showed that although vitrinite was the generator of metaplast in the thermoplastic stage, the expansion rate of vitrinite from coking coal is more than 70% greater than that from gas coal for two consecutive times. Moreover, the total weight loss of vitrinite from gas coal was about 1.262 times higher than that from coking coal, but the latter exhibited more generous aliphatic groups in pyrolysis products. In the thermal flow interval, the reaction activation energy of vitrinite and inertinite from coking coal and gas coal was 271.0 ± 0.7, 302.0 ± 1.5, 241.0 ± 0.1 and 300.25 ± 1.55 kJ/mol, respectively. Eventually, the kinetic and thermodynamic mechanism parameters of raw coal and macerals had favorable correspondence regularity, and macerals with the most prominent parameters would be dominant in the overall thermal properties of raw coal.

Cyclic Solid-Liquid Phase Transformations in the text {CaO}–text {SiO}_2 System—Experiments and Modelling

The cyclic growth and shrinkage of solid oxides (i.e. wollastonite) in text {CaO}–text {SiO}_2-based slags is investigated in-situ by means of High-Temperature Confocal Scanning Laser Microscopy (HT-CSLM). The compositions of the slags are carefully selected to induce different phase transformation conditions, i.e. congruent and incongruent melting/solidification. To complement the experimental results, the kinetics of growth and shrinkage of oxide crystals is investigated by means of a sharp interface model where the interfacial reaction and diffusion in the liquid bulk are considered as possible rate-controlling processes. The modelling approach combined with data analysis from key experiments reveals the underlying dissipative processes of solidification and melting phenomena, here, diffusion in the liquid bulk material and/or the interfacial reactions. The modelling approach is likely to be applicable for future materials design and processing problems from this perspective.

Decomposition of γ-Fe in 0.4C–1.8Si-2.8Mn-0.5Al steel during a continuous cooling process: A comparative study using in-situ HT-LSCM, DSC and dilatometry

Continuous cooling transformation (CCT) diagrams represent roadmaps for producing all heat-treatable steels. CCT curves provide valuable information on the solid-state phase transformation sequence, depending on the defined cooling strategies, the alloying concept of the steel and previous processing steps. The experimental characterization of CCT diagrams is usually done on a laboratory scale applying thermal analysis of dilatometry. In current research studies, however, also other in-situ methods such as high-temperature laser scanning confocal microscopy (HT-LSCM) or differential scanning calorimetry (DSC) are frequently used to investigate phase transformations during thermal cycling. In the present study, HT-LSCM observations and DSC analysis are critically compared with dilatometry results by investigating the CCT diagram of a 0.4%C-1.8%Si-2.8%Mn-0.5%Al (in mass pct.) advanced steel grade. Furthermore, classical examinations by optical microscopy and hardness measurements were performed to support the analysis. In general, very good consistencies between all experimental techniques were identified in determining the transformation start temperature for pearlite, bainite and martensite. The optical microscopy confirmed the observed phase transformations and the results correlated with the measured hardness response. Based on the results, coupling of HT-LSCM and DSC is considered as a valuable novel approach to plot CCT diagrams in future research.

The investigation of precipitation behavior of titanium compounds for high titanium steel based on in situ observation.

The effects of cooling rate, Ti content, and casting temperature on titanium compounds for high titanium steel were investigated. In-situ observation of high titanium steel during remelting and solidification was carried out by using a High Temperature Confocal Scanning Laser Microscope (HTCSLM), and the observed results were in good agreement with the thermodynamic and kinetic calculations. The observation and calculation results both show that the inclusions in high titanium steel first precipitate in the form of TiN, followed by TiC precipitates as temperature decreases, eventually forming TiCxN1-x type inclusions at room temperature. The initial precipitation temperature of the inclusions increases with the increase of Ti content in molten steel, whereas casting temperature has little effect on the initial precipitation temperature of inclusions. In addition, the size of TiN inclusions increases with the increase of Ti content in steel but decreases with the increase in cooling rate.

In-Situ Observation of Steel/Slag/Inclusion Interaction by Means of High-Temperature Confocal Scanning Laser Microscopy

Non-metallic inclusions (NMIs) in steels have been the focus of various experimental studies due to their detrimental character. While isolated processes, such as agglomeration or dissolution, have been well investigated, holistic in-situ views with high-temperature confocal scanning laser microscopy (HT-CSLM) have been rare. In this work a novel and suitable method is presented to simultaneously observe agglomeration, movement, detachment, and dissolution of non-metallic inclusions by combined the melting of steel and slag with a dual-crucible approach. Therefore, different steel/slag combinations were tested. It is shown that, with transparent that does not become tarnished by the ions stemming from the steel, the steel’s surface and non-metallic inclusions are observable. Furthermore, technological limitations are discussed, including restrictions regarding the melting point of steels and certain steel/slag combinations.

Grain boundary mobility of γ-Fe in high-purity iron during isothermal annealing

Grain boundary migration in pure electrolytic iron (Fe > 99.98 %) was studied under isothermal conditions at 1050 °C, 1150 °C, 1250 °C and 1350 °C. High-temperature laser scanning confocal microscopy (HT-LSCM) was used to observe the in-situ grain growth of austenite (γ-Fe) on the sample surface. The dependence of the arithmetic mean grain size on time and temperature were considered in a mathematical model according to classic grain growth theory. As no other effects, e.g., pinning by precipitation or impurity-induced solute drag, occur in pure Fe, the grain boundary mobility M was directly determined by fitting the experimental results. The temperature relationship followed an Arrhenius equation with M = 6.79*10−6*exp(-172750R−1T−1) m4J−1s−1. The mobility obtained differed by more than two orders of magnitude from Turnbull's postulation, which agreed with observations in the literature. The results matched published data extrapolated from a recent study on austenite grain growth in multicomponent steels.

In Situ Observation of Solidification and Crystallization of Low-Alloy Steels: A Review

Crystallization during the solidification process of steels is of vital importance for controlling the quality of final products. This paper summarizes the in situ characterization research activities of crystallization behaviors of low-alloy steels during the solidification process. The results obtained using high-temperature confocal laser scanning microscope (HT-CLSM) are critically reviewed, and other relevant methodologies, i.e., either classical method using differential scanning calorimetry (DSC) or large-scale facility (LSF), are also briefly mentioned. The evolution of the crystallization front from a planar to a cellular and further to a dendritic one, and subsequential microstructure evolutions, i.e., delta-ferrite (δ) formation from the liquid, austenite (γ) transformation and decomposition, are mainly discussed. The current review aims to highlight the state-of-the-art research outputs obtained by the novel in situ characterization techniques, and the obtained knowledge aims to shed light on the further development of the quality low-alloy steel products by controlling the processing and structure correlation.

Potential for carbide dispersive precipitation strengthening Ni-based alloy for high temperature

Increasing service temperature of wrought Ni-based superalloy by increasing alloying degree and fraction of γ′ phase has come to a bottleneck. In present work, an attempt is made to make maximum use of carbide to strengthen Ni-based alloy with a simpler chemical composition. Multiple morphology characterization methods and high temperature tensile test show that the newly designed Ni(bal.)-20Cr-0.80C–12Ta (wt%) alloy can be strengthened by TaC and Cr-rich M7C3 carbide and shows good ductility at 800 °C. Phase transformation characteristics detected by differential scanning calorimetry (DSC) and high-temperature confocal laser scanning microscopy (CLSM) images shows that there is a potential for dispersive precipitation of carbide in the alloy to get better mechanical property.

Effect of integrated austempering and Q&P treatment on the transformation kinetics, microstructure and mechanical properties of a medium-carbon steel

It is found that integrated bainite austempering with quenching & partitioning process is effective to refine microstructure and improve ductility of bainitic steels. However, the effect of this new processing route on the microstructure and mechanical properties as well as transformation kinetics of Q&P steels is not clarified. The present work investigates the effects of austempering and quenching & partitioning (AQ&P) process on the transformation kinetics, microstructure and mechanical properties of a medium-carbon steel by metallography, dilatometry, X-rays diffraction, high-temperature laser scanning confocal microscopy (HT-LSCM) and tensile tests. The bainitic transformation during partitioning was firstly dynamically observed with HT-LSCM. Results demonstrate that prior bainite formation before quenching was is effective to refine the microstructure, especially the blocky M/A islands emerged in mere austempering treatment and large-size tempered martensite induced by conventional Q&P process. In addition, compared to individual austempering or Q&P process, more retained austenite with higher carbon content, especially filmy retained austenite, was obtained by AQ&P process. Moreover, compared to individual austempering or Q&P process, mechanical properties were enhanced through pre-formed bainite in AQ&P process.

A new insight on the diffusion growth mechanism of intermetallic compounds in Al-Er system

The diffusion growth of intermetallic compounds in Al-Er alloys are closely related to the properties of the alloys. The current work aims at explaining the dominance of Al3Er in the Al-Er alloys precipitation phases and the interface thin layer phenomenon by diffusion couple technique, estimating the parabolic growth constant and diffusion activation energy of intermetallic compound in Al-Er diffusion couples to provide theoretical guidance for the design of new Al-Er alloys. In this work, Al-Er diffusion couples were successfully prepared by casting-cladding method in the atmosphere. The growth of Al-Er intermetallic compounds at diffusion couple interface during annealing were observed and recorded by High-Temperature Laser-Scanning Confocal Microscopy at 673, 698, 723 and 748 K respectively. The results show that the growth characteristics of Al-Er intermetallic compounds were accord with layer-terraced growth during annealing. The thickness of intermetallic compound was linear with the square root of time at experimental temperature. The intermetallic compound layer was composed of Al3Er and a very thin AlEr phase. The parabolic growth constants of Al3Er phase at 673, 698, 723 and 748 K were 1.017 × 10−14, 1.609 × 10−14, 3.111 × 10−14 and 4.76 × 10−14 respectively. The activation energy of Al3Er phase was (88.4 ± 5.3) kJ/mol and the pre-exponential factor was 7.126 × 10−8 m2/s.

In-situ observations of solidification process of Fe–Al–Ta eutectic alloy

The Fe–Al–Ta eutectic alloy can be formed by eutectic reaction in order to improve the performance of Fe–Al intermetallic compounds, and thus it is important to further clarify the crystal growth mechanism of the Fe–Al–Ta eutectic alloy during solidification. Thus, the melting and solidification temperatures of the Fe–Al–Ta eutectic alloy were determined by differential scanning calorimetry, and the melting and solidification processes of the Fe–Al–Ta eutectic alloy were observed in situ by high-temperature confocal scanning laser microscopy. In addition, the solidified structure of the Fe–Al–Ta eutectic alloy was observed and characterized by scanning electron microscopy and energy dispersive spectroscopy. No other types of phase transitions were found in the Fe–Al–Ta eutectic alloy when the temperature was below 1600 °C. The reinforced phase exhibited a certain orientation after solidification, and the microstructure at the center of the eutectic cell was much more regular than that at the grain boundary. The effect of the cooling rate on the microstructure morphology and the formation mechanism of the irregular divorced eutectic were analyzed.

Agglomeration behavior of rare earth inclusions and alumina inclusions at the interface between argon and molten steel

Nozzle clogging frequently occurs in steel containing rare earth (RE) due to the aggregation of RE inclusions, which seriously interferes with the application of RE in steel. To provide insights into nozzle clogging, the agglomeration behavior of inclusions in RE-containing steel was investigated by laboratory experiments and theoretical calculations. High-temperature confocal laser scanning microscopy (HT-CLSM) was applied to observe the behavior of inclusions at molten steel surfaces and their interactive forces. Kralchevsky–Paunov (K–P) model was used to predict the capillary force acting on different inclusions. The results show that the interactive forces that acted on inclusions were investigated as a function of inclusion size, inter-distance, and inclusion composition. It is found that the capillary force acting on the inclusions decreases in the order of Ce2O3 > CeAlO3 > Al2O3. This study verified the applicability of the K–P model in RE-containing steel, which can provide theoretical support to help solve the nozzle clogging problem during rare earth steel production.