M23C6 Carbides Research Articles

Qualitative study of carbides in liquid phase sintered M3:2 high speed steel

The microstructure of liquid phase sintered M3:2 high speed steel and the effect of adding carbon and silicon on the microstructure was characterized by scanning electron microscopy, dispersive spectrometry, and X-ray diffraction. Various types of carbides were formed depending on the added carbon and/or silicon, the sintering atmosphere and the cooling rate. The microstructure of sintered M3:2 high speed steel samples in vacuum conditions without the addition of Si and graphite is composed mainly of MC and M6C carbides inside cells and primarily at cell boundaries. The M2C eutectic carbides in these samples were formed at cell boundaries and their amounts and morphology depends on the cooling rate. Sintered samples in N2 atmosphere with added carbon and silicon, M6C eutectic and M7C3 eutectic carbides were dominantly formed while carbonitrides were formed in smaller amounts.

Effect of the Mn and Cr contents on the oxidation and creep resistance at 1100°C of cast cantor–based HEAs

Cast High Entropy Alloys (HEAs) derived from the Cantor’s composition may represent alternative substitutional solutions to the superalloys which are constituted for more than half of the critical elements nickel and cobalt. Recently, MC–alloyed HEAs constituted by a Cantor’s type matrix associated to an efficient interdendritic network of MC carbides, have demonstrated promising creep resistance at elevated temperatures. Regrettably, they also show poor high temperature oxidation resistance. This bad oxidation behavior is possibly due to the deleterious effect of manganese and to a too low content in chromium. New alloys were elaborated and tested in oxidation at 1100°C with thermogravimetry follow–up and metallographic characterisation, and their creep behavior was controlled. With less Mn and more Cr than the original alloys, these new alloys demonstrated significant progress in oxidation resistance. These changes in chemical compositions did not modify their creep resistances which were globally maintained, for the carbide-free alloy as well as for the MC-containing ones. These Mn-decreased and Cr-increased MC-containing alloys can be considered as low-cost alternative to polycrystalline Ni or Co-based superalloys for working in moderate conditions of corrosive fluids and applied mechanical stresses.

Solidification path and precipitation mechanism of a Ni-Cr-co-Mo based heat-resistant alloy

The solidification path and precipitation mechanism of the C-HRA-3 Ni-Cr-Co-Mo-based heat-resistant alloy are investigated by methods such as differential scanning calorimetry analysis, in-situ observations, quenching experiments, and scanning transmission electron microscopy. The results confirm that the primary solidification precipitates in the center of the C-HRA-3 alloy VAR ingot consist of Ti(C,N), M6C-M23C6 symbiotic phases, Ti(C,N)-M6C-M23C6 symbiotic phases and surrounding dispersed M6C and M23C6 carbides. The precipitation temperatures for Ti(C,N), M6C, and M23C6 are 1310 °C, 1280 °C, and 1230 °C, respectively. The C-HRA-3 alloy exhibits a wide solidification temperature range of 176 °C (1390 °C ∼ 1214 °C). Within 1390 °C ∼ 1355 °C, the γ phase grows vigorously, accompanied by a significant reduction in the fraction of liquid phase. At 1355 °C ∼ 1214 °C, the decrease in liquid phase fraction slows down, accompanied by significant enrichment of Mo, Cr, C and Ti elements. There is a clear functional relationship between the liquid phase percentage and temperature. M6C carbides undergo two heterogeneous nucleation mechanisms in the liquid phase. Due to the degradation of M6C carbides discharging Cr and C atoms, M23C6 carbides form at their edge. Dispersed M6C and M23C6 carbides nucleate at misfit dislocations around the symbiotic phases. Appropriately reducing the cooling rate during the stage above the precipitation temperature and increasing the cooling rate below the precipitation temperature can significantly reduce the volume percentage and size of the symbiotic phases.

Creep cavities and carbide evolution in interrupted creep conditions along P91 steel of dissimilar weld joint

The creep behaviour of dissimilar weld joint of 316LN SS-P91 steel when subjected to lower applied stresses (below 100 MPa) generally fails in a Type-IV pattern. The dissimilar weld joint was welded through shielded metal arc welding (SMAW) process with INCONEL as electrode, a nickel-based superalloy. An interrupted creep test was carried out at creep condition of 80 MPa −600 °C temperature. Interruption was done at two stages of creep, i.e. (a) mid of secondary and (b) start of tertiary. Microstructural evolution with respect to the hardness variation along various regions of P91 steel at interrupted and the failed specimen was done. A coarsening of hierarchical boundaries and M23C6 carbides was observed along HAZ region that has resulted with respect to time and temperature.

Effect of long-term thermal aging on lead-bismuth eutectic corrosion behavior of 9Cr ferritic/martensitic steel

In lead-cooled fast reactor (LFR) systems, the liquid lead-bismuth eutectic (LBE) coolant provides a corrosive environment that damages the steel components during high-temperature operation. This study investigated the microstructural deterioration of 9Cr ferritic/martensitic (F/M) steel under thermal aging at 550 °C for 2,000, 10,000, or 20,000 h and its effect on oxidation corrosion in an LBE environment using multiscale characterization techniques. The results indicated that the thickness of the internal oxidation zone (IOZ) increased significantly with extended thermal aging, whereas that of the spinel layer remained relatively constant. The abundant subgrain boundaries that emerged during extensive thermal aging facilitated Fe diffusion, and the enlarged Cr-rich M23C6 carbides contributed to the formation of preferential oxidation regions, accelerating IOZ layer growth. The spinel layer formed from the IOZ was influenced by microstructural defects within the IOZ. A theoretical model describing the accelerated oxide layer growth due to thermal aging was developed. These findings support the advancement of LFR technology.

Optimization and high-temperature wear characterization of Stellite alloy claddings developed using TIG welding on 56NiCrMoV7 die steel

In this study, Stellite 6 and Stellite 12 claddings were deposited on 56NiCrMoV7 hot-worked die steel using the Tungsten Inert Gas (TIG) welding process. Initially, single tracks were deposited using a full factorial design varying two process parameters - current (65, 75, and 85 A) and scan speed (400, 600, and 800 mm/min). The single tracks were then optimized based on dilution rate and microhardness. The optimized parameters were used to develop Stellite 6 and 12 multi-pass clad layers on 56NiCrMoV7. The evaluation of the microstructure of the claddings was done using an optical microscope, XRD, FESEM, EDX, and EBSD. The microstructure of the claddings consists of α-Co matric with M7C3, M23C6, and W2C carbides precipitated along the grain boundaries. Further microhardness and tribological performance were analyzed using Vicker's hardness tester and ball-on-disc tribometer, respectively. Stellite 12 claddings exhibited superior wear resistance and indicated reduced wear volume by 51.3 % at room temperature, 69.2 % at 450 °C, and 32 % at 550 °C compared to the base material and 53.2 % at room temperature, 37.3 % at 450 °C, and 24.1 % at 550 °C compared to Stellite 6 claddings. The KAM mapping showed higher dislocation density for Stellite 12 cladding. The combination of finer grains, higher hardness, and higher dislocation density resulted in higher wear resistance.

Study on the characteristics and high-temperature dissolution mechanism of eutectic carbides in medium-alloy steel

In this study, the high-temperature evolution of eutectic carbides in a medium-alloy steel was investigated as well as their precipitation mechanism. Results revealed that MC and M6C eutectic carbides in the steel appeared during the final solidification due to the segregation of Mo and V and the melt undercooling. These eutectic carbides consist of blocky shapes with varying orientations, and rod-like shapes with the same orientation. Further investigation was confirmed that the carbides (MC and M6C) exhibited an intergrowth behavior. The cooling rate had a direct influence on the secondary dendrite arm spacing (SDAS), which decreased from 180 to 130 μm as the rate ranged from 0.6 to 21.9 °C/min. After holding for 0, 25, 50, and 80 h, respectively, the volume percentage of eutectic carbides exhibited a significant decreasing trend from 2 to 0.2%. Additionaly, the carbides exhibited irregular morphology after holding for 0–50 h, respectively, and which was transformed into the rod-like shape with a small size distributed along the grain boundaries after holding for 80 h. This phenomenon was attributed to the mutual diffusion between Mo, V, and other alloying elements in the carbides and Fe element in the steel matrix.

Effect of Inconel 718 Filler on the Microstructure and Mechanical Properties of Inconel 690 Joint by Ultrasonic Frequency Pulse Assisted TIG Welding.

Ultrasonic frequency pulse assisted TIG welding (UFP-TIG) experiments were conducted to join Inconel 690 alloy (IN690) by adding Inconel 718 alloy (IN718) as the filler. The effect of the filler on the microstructure, mechanical properties, and ductility dip cracking (DDC) susceptibility of IN690 joints were investigated. The results show that a variety of precipitates, including MC-type carbide and Laves phases, are formed in the weld zone (WZ), which are uniformly dispersed in the interdendritic region and grain boundaries (GBs). The increase in the thickness of the IN718 filler facilitates the precipitation and growth of Laves phases and MC carbides. However, the formation of Laves phases in the WZ exhibits a lower bonding force with the matrix and deteriorates the tensile strength of IN690 joints. Due to the moderate content of Laves phases in the WZ, the IN690 joint with 1.0 mm filler reaches the maximum tensile strength (627 MPa), which is about 96.5% of that of the base metal (BM). The joint with 1.0 mm filler also achieves the highest elongation (35.4%). In addition, the strain-to-fracture tests indicate that the total length of cracks in the joint with the IN718 filler decreases by 66.49% under a 3.8% strain. As a result, the addition of the IN718 filler significantly improves the mechanical properties and DDC resistance of IN690 joints.

Effects of annealing powder on microstructures and tensile properties of LPBF-processed Haynes230 superalloy

ABSTRACT This study reveals a novel understanding of the influence of annealing the feed powder, which alters the precipitate characteristics in the powder particles on the microstructure and mechanical properties of Haynes230 superalloy fabricated by laser powder bed fusion (LPBF) plus hot isostatic pressing (HIP) and solution treatment. Specifically, annealing Haynes230 superalloy powder at 1000°C for 1 h under vacuum resulted in the precipitation of M6C carbide instead of the typical M23C6 found in unannealed powder. The alloy fabricated by LPBF of the annealed powder plus HIP and heat treatment exhibited an increased number density of the carbide precipitates at grain boundaries, but a reduced number density of the intragranular carbide precipitates. Consequently, its ambient temperature tensile properties decreased clearly in terms of yield strength (406–383 MPa), ultimate tensile strength (936–841 MPa) and elongation to fracture (38.6% to 25%) compared to the alloy fabricated by LPBF of the as-received powder plus same post-print processing. However, the annealing of the feed powder had little effect on the tensile properties of the samples at 900°C. These findings underscore the significant impacts of feed powder microstructure on the mechanical properties of LPBF-processed superalloys.

Effect of C content on microstructure evolution and mechanical properties of CoCrFeNiTa0.1 high entropy alloy

A series of CoCrFeNiTa0.1Cx (x = 0.1, 0.2, 0.3, 0.4, 0.5) high entropy alloys (HEAs) with different C content were prepared by vacuum melting technology. The influence of different C element contents on the alloy microstructure and mechanical properties have been systematically investigated using X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and a universal testing machine system. It is found that the introduction of trace amounts of C element content facilitates the precipitation of Laves phase in C0.1 alloy. As the C element content further increases, the volume fractions of both FCC matrix and Laves phases gradually decrease, while the volume fraction of M7C3 carbide increases. Notably, the CoCrFeNiTa0.1C0.3 HEA shows a ternary eutectic structure. Compression tests reveal an increase in yield strength from 342 MPa to 1475 MPa and hardness from 182 HV to 458 HV as the C content increases. The precipitation of Laves phase and M7C3 carbide is principally involved in the enhancement of strength and hardness. Nanoindentation tests indicate that the M7C3 carbide has a higher nano-hardness compared to FCC matrix and Laves phase. The fracture microstructure exhibits a mode transition from ductile fracture to cleavage fracture.

Effect of heat treatment on the anisotropic mechanical properties and corrosion resistance of laser powder bed fusion fabricated Inconel 625

The microstructure evolution of laser powder bed fusion processed Inconel 625 after heat treatment at 650 ℃ (aging), 850 ℃ (sensitization) and 1050 ℃ (homogenization) was studied. Relationship of microstructure evolution and the anisotropic mechanical properties and corrosion resistance was analyzed. Decreased corrosion resistance after aging and sensitization was observed, which is related to the different precipitation behavior. After aging, γ″ and MC carbides precipitated along cellular structures further accelerate the corrosion along melting pool boundaries. While after sensitization, δ precipitated along cellular structures aggravated the corrosion along the melting pool boundaries. At the meantime, precipitation of M23C6 carbides and δ along grain boundaries made it vulnerable to be corroded, which further accelerate the corrosion rate. After homogenization, segregation and precipitates are barely observed in the microstructure which contribute to an enhancement of corrosion resistance. Moreover, with the increasing of heat treatment temperature, recovery of anisotropic microstructure contributes to the decrease of the anisotropy of mechanical properties. This study may contribute to the profound comprehension of heat treatment procedure on microstructure evolution as well as mechanical properties and corrosion resistance of laser powder bed fusion processed Inconel 625.

Effect of PWHT on microstructure and mechanical properties of welded joint of a new Fe-Ni-based superalloy

In this study, the effect post weld heat treatment (PWHT) on microstructural evolution and mechanical properties of weld metal of HT700P alloy with Inconel 617 filler metal was investigated. After welding, columnar grain, dendritic microstructure and segregation of Mo, Co and Ti elements related to the equilibrium distribution coefficient were observed in the weld metal. The PWHT was conducted in both direct-aging treatment with different time and solution treatment with different cooling methods. The results showed that direct-aging treatment had a limit impact on homogenization of weld metal, while microstructural homogenization and elemental segregation were significantly improved after solution treatment and massive M6C and M23C6 carbides precipitated at the grain boundaries and interdendritic region of weld metal. It was found that the elongation at 700 °C of welded joints after solution treatment was relatively increased, which was related to the decrease of residual stress and the precipitation of Mo-rich carbides at the grain boundaries. The fracture occurred in the weld metal presented interdendritic fracture characteristics, and the fracture mechanism for stress relaxation cracking was the strong grain interior induced by the precipitation of γ′ phase, leading to the stress concentration and nucleation of cavities at grain boundaries. After solution treatment, the creep lifetime of furnace cooling was much greater than that of water quenching. The superior creep properties of furnace-cooled joint could be attributed to the lower residual stress and the migration of carbon element in the fusion line, which inhibited the nucleation and aggregation of cavities in the partially melted zone.

Microstructural Analysis of K-TIG-Welded New Ni-Based Superalloy VDM Alloy 780

The fusion zone microstructures in K-TIG-welded and post-weld solution heat-treated new superalloy VDM Alloy 780 were examined. In addition, the kinetics of the base metal grain growth during solution heat treatments were analyzed. (S)TEM analyses show that major interdendritic microconstituents formed in the fusion zone due to elemental microsegregation are MC carbides and coarse irregularly shaped Laves phase. Additionally, minor secondary interdendritic phases are found to include γ′, γ″, and tiny plate-like Laves particles. To prevent any potential deterioration of mechanical properties caused by the irregular Laves phase, post-weld solution heat treatments (PWSHTs) at 954 °C to 1060 °C/1 hours were performed to remove the Laves phase. PWSHT at 954 °C only partially eliminates the Laves particles while forming an abundance of interdendritic δ/η phase. Laves phase is dissolved entirely without forming δ/η platelets after PWSHT at 1060 °C. It is proven that Laves eutectics in VDM Alloy 780’s fusion zone can be eliminated through PWSHT without significantly coarsening the base metal’s grain size in comparison to Alloy 718 as a result of substantial grain growth inhibition likely caused by solute segregation at grain boundaries.

Heterogeneous microstructure and mechanical properties of carbon-doped FeCoCrNiMn high-entropy alloy

Heterogeneous microstructure with nano-precipitate and bimodal grain size distribution was obtained in a FeCoCrNiMn high-entropy alloy (HEA) doped with 0.5 at.% C by a controlled thermo-mechanical treatment. The coarse M23C6 carbides tend to aggregate along the fine grain boundaries. Compared to the sample with homogenous microstructure, the heterostructure FeCoCrNiMn−0.5at.%C HEA has approximately the same average grain size of 4.8 μm. However, it shows bimodal grain size distribution and higher volume fraction of the fine grains (<3 μm), resulting in the increase of yield strength from 552 to 632 MPa. The sample with heterostructure presents different mechanical responses and deformed microstructures in different regions, accounting for significant strain localization and high density of the geometrically necessary dislocations during tensile deformation. These deformation characteristics are beneficial to the enhancement of strain hardening capacity, thereby promoting strength−ductility synergy.

Synergistic influence of cerium and yttrium micro-addition on microstructure and mechanical tensile properties of K465 nickel based superalloy

The microstructures and room temperature tensile properties of a nickel-based cast superalloy K465 were investigated with the cerium (Ce) and cerium + yttrium (Y) additions, respectively. In K465 superalloys, Ce element was found to distribute in the internal grains of K465. And, the Y element was shown to combine towards with the MC carbides. The tensile properties experienced increasement with the addition of Ce and Y, 0.86 % increasement for Ce addition and 8.35 % increasement for Ce + Y addition. The synergistic effect of rare earths element plays a positive role in the mechanical properties of the nickel based superalloy.

Relating rolling contact fatigue (RCF) life to the microstructure evolution in aerospace grade bearing steels: A comparison of Cronidur-30 with AISI 440C

This article presents an extensive analysis of the microstructural evolution under various heat treatment conditions, mechanical properties (hardness), and rolling contact fatigue (RCF) life assessment and sub-surface crack analysis are studied on high nitrogen bearing steel Cronidur-30(Cr-30). An optimum solutionising temperature range has been identified which ensures desirable hardness as well as low retained austenite content. The microstructure consists of primary M2 (C, N) and secondary M23C6 carbides. Sizes of carbides in Cr-30 are significantly smaller than in AISI 440C and this plays a critical role in enhancing the RCF life of Cr-30. A larger area fraction of fine carbides results in branches and subsequent sub-branches of cracks in Cr-30 steel. However, the AISI 440C sample exhibits extensively interconnected cracks due to the presence of larger carbides. The tempering response of Cronidur-30 exhibited a peak hardness of 61 HRC at both lower (150 °C) and higher (475 °C) temperatures. Higher temperature tempering showed L1 life improvement of over 0.5 fold compared to lower temperature tempering.

Carbide Precipitation Behavior of High‐Alloy Steel During Solidification and Cooling Process

The precipitation, growth, and transformation of carbides rich in Cr and Mo during solidification and cooling process of high‐alloy steel for cold working dies are investigated. The Fe–C pseudobinary phase diagram of high‐alloy steel is calculated by Thermo‐Calc software to ascertain the critical phase transformation temperatures. The temperatures of phase transformation during the solidification process are determined by a differential scanning calorimeter. Then the microstructure of the samples at these characteristic temperatures is observed in situ by high‐temperature confocal microscope. The results show that the characteristic temperatures for phase transformation and carbide precipitation are 1380, 1315, 1140, and 980 °C, respectively. At 1315 °C, thick rod‐like or island‐like M7C3 carbides enriched in Cr and Fe are formed. At 1140 °C, secondary M7C3, adhering to the primary eutectic M7C3, grows rapidly in a rod‐like morphology and maintains a similar composition. The secondary M6C carbides of segregated Mo elements precipitate in fan‐shaped clusters near M7C3 through the dissolution of M7C3 and the conversion of M2C. Thermodynamic calculation further indicates that the eutectic Cr7C3 precipitates at 1213 °C, and secondary Cr7C3 remains under conditions favorable for precipitation below the solidus, preceding the precipitation of secondary carbides Cr23C6 and Mo2C.

Delayed recrystallization behavior and deformation mechanism of IN738LC alloy prepared by laser powder bed fusion

The design and development of heat treatment regimes adapted to the laser powder bed fusion technology for specific service conditions have become a hot topic of research in the field of additive manufacturing. This paper systematically studies the microstructure changes of the L-PBFed IN738LC alloy, solution heat treated at 1250 °C for various durations (1 h, 3 h, 5 h) and then aged at 850 °C for 24 h. The delayed recrystallization behavior was revealed, and the selective precipitation pattern of the M23C6 carbide on different types of grain boundaries was discussed. Additionally, the tensile deformation mechanism of the alloy before and after heat treatment is clarified. The results indicate that grain boundary migration and transformation are impeded under 1250 °C/1 h conditions due to carbide particle pinning and solute atom segregation during the initial stage of solution treatment, which accounts for the delayed recrystallization behavior, and the microstructure is mainly undergoing recovery. At 1250 °C/5 h, M23C6 carbides selectively precipitate at twin boundaries, accompanied by recrystallization. The samples treated at 1250 °C/1 h exhibit the highest mechanical property (σYS=1305 ± 21 MPa, σUTS=1462 ± 11 MPa, εEL=5.4 ± 0.7 %) owing to the precipitation of γ′ phase and the presence of sub-grain boundaries. The deformation mechanism shows that the as-built samples mainly experience planar dislocations slipping, while the heat-treated samples undergo stacking faults shearing and anti-phase boundary shearing. The dominant mechanism among these is anti-phase boundary shearing.

Tensile and creep resistance improvement of GH4975 alloy for turbine discs via electron beam smelting layer solidification technology

A difficult-to-deform superalloy for turbine disks, which can be used at 850 °C for a long time, was prepared by electron beam melting layer solidification (EBSL) technology with high purity and fine structure. Subsequently, the ingot was processed by hot extrusion technology instead of conventional hot forging, and then the tensile and creep tests were performed after standard heat treatment. The results show that the EBSL alloy exhibits excellent high-temperature strength and creep rupture life compared to the conventional preparation method. Among them, the yield strengths at 20 °C and 850 °C are 8.1 % and 5.2 % higher than those in the literature, and the creep rupture life at 850 °C and 412 MPa is 1.53 times higher than that in the literature. The dislocation-precipitate interaction reveals that dislocation shearing γ′ phase is the major mechanism at 20 °C and 850 °C tensile, and Orowan looping and stacking fault shearing are the decisive mechanism during creep at 850 °C and 412 MPa. MC carbides remaining during solidification are the main source of cracks during deformation by fracture analysis. The reasons for refining the microstructure and improving the purity by electron beam melting are analyzed and explained. We believe this work can provide new ideas and methods for preparing superalloys.

Study on the tensile properties and deformation mechanism of high-temperature resistant nitrogen-containing nickel-based welding material deposited metal

This article uses a new type of nitrogen-containing nickel-based flux cored welding wire as the experimental material to study the tensile properties and deformation mechanism of the deposited metal from room temperature to 900 °C. The results show that the tensile strength gradually decreases with the temperature. The plasticity gradually increases, but the lowest value appears at 700 °C, which is the phenomenon of intermediate temperature brittleness. M23C6 carbides begin to decompose at 700 °C. More carbonitrides are precipitated within the crystal with temperature. In the low-temperature zone (T ≤ 600 °C), the main deformation mechanism is the unit dislocation a/2<110> cutting precipitation phase. In the medium-temperature zone (600 °C < T ≤ 750 °C), initiation of Orowan bypass mechanism for dislocations. In the high-temperature zone (800 °C ≤ T ≤ 900 °C), the slip and climbing mechanism of dislocation is the main deformation mechanism.