Microstructural Evolutions During Thermal Aging of Alloy 625: Impact of Temperature and Forming Process

The microstructural evolutions occurring upon thermal aging of alloy 625 sheets were studied in the 823 K to 1173 K (550 °C to 900 °C) temperature range and for durations up to 2000 hours. TTT diagrams of the δ and γ″ phases were established based on high-resolution scanning electron microscopy and associated quantitative image analysis approaches. The evolutions of secondary carbide volume fraction were also characterized. It was observed that the precipitation domains of the γ″ and δ phases are, respectively, 823 K to 1023 K (550 °C to 750 °C) and 923 K to 1173 K (650 °C to 900 °C) and that the γ″ coarsening follows the LSW theory once these particles have an ellipsoidal morphology. The onset of grain growth, accompanied with an increase of the texture index, was observed at a temperature as low as 1173 K (900 °C). It results from the progressive dissolution of grain boundaries’ secondary carbides (especially M₆C carbides) at this temperature, a process that favors a greater mobility of grain boundaries. It is also shown that the forming process (shear spinning), even after a relaxation heat treatment, enhances and stabilizes the precipitation of the δ phase compared to as-rolled + solution heat-treated sheets. It hence slows down the precipitation of the γ″ phase, a result that is in good agreement with a thermal aging that was performed under load (i.e., during a creep test).     

GH4710合金的相析出特征及其与热加工塑性损伤的关联性

利用Thermal Calc热力学软件、光学金相显微镜、扫描电镜等手段分析了GH4710合金原始态和不同条件热物理模拟变形后的析出相及加工损伤特征,系统研究了析出相特征与该合金热加工塑性损伤及开裂的关联性.结果表明:GH4710合金的原始组织主要由γ'、MC及M₂₃C₆碳化物、γ+γ共晶组织组成;热加工时微孑洞等损伤在MC碳化物及γ+γ共晶组织处形核后沿晶界扩展,最终相互连接导致合金大面积破坏;γ'相优先在MC碳化物及共晶组织附近析出,并通过其共格应力场的作用增加了损伤形核和扩展阻力,使合金在较低温度下的塑性损伤值明显小于高温条件下.      

Microstructure characteristics of spray-formed high vanadium and cobalt high speed steel

The microstructure of high vanadium and cobalt high speed steel(high-V/Co HSS) and the morphology of its carbides were analyzed by optical microscope(OM),scanning electron microscope(SEM),electron probe microanalysis(EPMA),X-ray power diffraction(XRD),atomic force microscopy(AFM) and single phase erosion(SPE).The results suggest that the as-sprayed high-V/Co HSS has fine equiaxed grains(about 20 μm in size),which were homogeneously distributed.The carbides have two classical morphologies:one is fine particles(about 2 μm in size) distributed along the grain boundaries and the other is needle-like one,distributed on the grain boundaries.There are MC carbides,M2C carbides,M6C carbides and Cr2WC2 carbides in the as-sprayed high-V/Co HSS samples,however,in the as-cast high-V/Co HSS,there are MC carbides and Cr2WC2 carbides only.The SPE results show that there are two types of MC carbides in the as-sprayed HSS:the sphere one and the particle-like one.The former is about 2 μm in size and the latter is less than 1 μm,dispersed inside the grains,quite different from the MC carbides in the as-cast HSS.According to the AFM results,the skeleton-like M6C carbides of the as-sprayed high-V/Co HSS are embedded in the matrix along the grain boundaries.It is found that there are sharp membrane pieces on the carbides.Some small bamboo-shoot-like MC carbides grow from the matrix and are dispersed inside the grain.Those larger MC carbides are spherical particles embedded at the grain boundary junctions.     

The influence of applied stress and stress sense on grain boundary precipitate morphology in a nickel-base superalloy during creep

Creep induced instability of strengthening precipitates at grain boundaries is of general concern in the applications of many high temperature alloys. Having shown that the general validity of the existing mechanism for such an instability in nickel-base superalloys may be considered suspect, this paper reports and discusses the effects of both tensile and compressive creep on γ′ grain boundary precipitate morphology in an alloy consisting of γ′ (Ni₃Al) precipitates in a γ (nickel solid solution) matrix. We find that the uniform distribution of γ′ precipitates is altered by the application of uniaxial creep stress, with the stress-induced precipitate morphology depending strongly on stress sense. Tensile creep results in the dissolution of γ′ precipitates at grain boundaries aligned more or less transverse to the stress axis, with an accompanying increase in volume fraction of γ′ precipitates at grain boundaries oriented parallel to, or almost parallel to the stress axis. In contrast, the reverse change in morphology occurs during compressive creep. The observed morphology changes and their dependence on stress sense are shown to be consistent with the flow of chromium atoms from grain boundaries that are under normal compression towards grain boundaries that are under normal tension. The results conclusively demonstrate that Herring-Nabarro type diffusion in multiphase, polycrystalline alloys can cause chemical changes in grain boundary regions which, in the extreme, result in phase changes at grain boundaries. The results and proposed mechanism are discussed in terms of the findings of other investigations.     

Microstructural evolution and mechanical properties of a new Ni-based heat-resistant alloy during aging at 750℃

Microstructural evolution and mechanical properties of a new candidate Ni-based heat-resistant alloy for advanced ultra-supercritical( A-USC) steam turbine rotors were investigated during aging at 750 °C up to 10 000 h. The evolutions of γ' particles inside austenitic grain and M_(23)C_6 carbides along grain boundaries were characterized according to their morphologies,distributions,and growth kinetics. Mean radius of the γ' spherical particles grew from 20. 3 to 90. 0 nm after aging for 10 000 h,and the corresponding coarsening behavior was conformed to the law of Lifschitz-Slyosovd-Wagner( LSW). The weight fraction of γ' particles slightly increased from 10. 0 to 12.0wt. % after aging of long duration at 750 ℃. The Cr-rich M_(23)C_6 carbides discontinuously precipitated along grain boundaries,while other detrimental phases were not formed during the aging treatment,and hence the strength of grain boundary was enhanced by these discontinuously distributed carbides. The critical size of γ' had a direct influence on the maximum hardness of this alloy. Moreover,this alloy presented a good impact toughness for the safety after long time aging at high temperature.     

熔体过热处理对K465合金晶粒和碳化物的影响

 研究了用CaO坩埚真空感应熔炼、再经不同的熔体过热处理后,K465铸造高温合金晶粒尺寸的变化以及合金中碳化物的形貌和分布特征。结果表明：在浇注温度相同的条件下,未经熔体过热处理时,合金晶粒为普通等轴晶,碳化物为块状MC碳化物;熔体过热处理温度在1 600~1 750 ℃之间时,晶粒尺寸随处理温度升高而长大,〖JP2〗初生MC碳化物从块状转变为汉字草书体群团形式,而且呈现出温度升高,MC碳化物变细、群团变小的趋势;过热处理温度超过1 750 ℃时,草书体群团MC碳化物随温度升高晶粒尺寸不断减小并呈细小点状均匀分布。     

Inconel 690合金TT处理后的析出相

 用扫描电子显微镜、透射电子显微镜和相分析研究了3种不同钛含量的Inconel 690合金经不同固溶温度+715 ℃×15 h,TT处理后的析出相。结果表明：合金经TT处理后,均有M23C6析出,并含有一定量的Ti(C,N);钛含量为110%的合金中有γ′相析出,γ′相在晶内弥散分布;M23C6大多在晶界上析出,而且在孪晶界和晶内位错线处也均有析出,M23C6与界面一侧基体保持立方 立方的平行位向关系;钛含量增加,析出的M23C6尺寸变小,间距增大,晶界附近的铬含量明显提高,有利于改善合金的耐腐蚀性能。     

Grain growth and carbide precipitation in superalloy, UDIMET 520

The results of an experimental study on the grain coarsening behavior, M₂₃C₆ carbide precipitation, and secondary MC carbide precipitation kinetics in UDIMET 520 are presented. Primary MC carbides and M (C, N) carbonitrides strongly influence the grain growth, with their dissolution near 1190 °C and 1250 °C, respectively, resulting in two distinct grain coarsening temperatures (GCTs). M₂₃C₆ carbides precipitate in the alloy over a wide range of temperatures varying between 600 °C and 1050 °C. A discrete M₂₃C₆ grain boundary carbide morphology is observed at aging temperatures below 850 °C. Secondary MC carbides formed at temperatures ranging between 1100 °C and 1177 °C, in specimens in which primary MC dissolution had been obtained at solution treatment temperatures of 1190 °C to 1250 °C. A schematic time-temperature-transformation (TTT) diagram for understanding the microstructure and precipitation inter-relationships in UDIMET 520 alloy is also presented.     

The initiation of intergranular failure in inconel-600

The nature of slip interaction with the grain boundaries was examined on the polished surface of Inconel-600 pulled in tension at 370°C and at the initial strain rate of 1.65 × 10^?6 sec^?1. It was shown that the grain boundaries could not always accommodate slip taking place at the boundary regions. This led to the separation of grains at the boundary. Depending on the detailed morphology of the carbides, these intergranular cracks could form at axial strains as low as 10 pet. Since the cracking takes place in the inert atmosphere, it is concluded that the grain boundaries are inherently embrittled by the formation of carbides and/or by solute segregation. There was no evidence of grain boundary sliding, but when carbides were absent highly localized slip in the boundary region gave the appearance of grain boundary offsets. The implications of these observations to stress corrosion cracking are discussed.     

The influence of electron-beam welding parameters on heat-affected-zone microfissuring in INCOLOY 903

The microfissuring in the heat-affected zone (HAZ) of electron-beam-(EB-) welded thermomechanically processed INCOLOY 903 has been studied with a view to reducing the incidence of microfissuring and to obtaining a better understanding of the influence of EB welding parameters on it. For a given heat of material, microfissuring susceptibility has been quantitatively related to EB welding parameters and the shape of the weld pool. Fractional factorial experimental study of welding parameters showed that a reduction in welding speed and an increase in EB current for a given heat input would minimize HAZ microfissuring in the alloy. It was observed that with lower travel speeds, bccause of the shallower temperature gradients in the HAZ, the amount of liquated grain boundary area is less, thus leading to decreased microfissuring. Considerable HAZ microfissuring was observed on the coarse grain boundaries of warm-worked grains. The microfissures appeared to initiate in regions slightly removed from the fusion line. Minimal microfissuring was observed on the grain boundaries of fine recrystallized grains. These boundaries, however, had a thickened appearance bccause of the formation of Nb-enrichedy phase by the process of grain boundary liquid film migration (LFM). The origin of the liquid on the grain boundaries is suggested to be due to the constitutional liquation of preexisting primary carbides (partial), fine MC carbides, and MNP-type phosphides. It is suggested that substantial occurrence of LFM in the HAZ minimizes microfissuring by decreasing the total temperature range of solidification and also by enabling the grain boundary liquid to solidify without the occurrence of low-melting terminal eutectic reaction.     

Microstructural characterization of INCOLOY 903 weldments

The fusion zone and the heat-affected zone (HAZ) microstructures obtained during electron beam welding of thermomechanically processed INCOLOY 903 have been characterized by analytical electron microscopy. The microsegregation observed during solidification in the fusion zone indicates that while Fe and Co segregate in the gamma dendrites, Nb, Ti, and C are extensively rejected into the interdendritic liquid. Electron diffraction and energy dispersive X-ray microanalyses on secondary phases extracted from the fusion zone, from the HAZ microfissures, and from the HAZ grain boundaries on carbon replicas established the major secondary solidification constituent formed from the interdendritic liquid to be cubic niobium-rich MC carbides. Laves phase was observed only in trace amounts. Continuous sheets of the MC carbides were observed in the HAZ grain boundary microfissures, while the HAZ grain boundaries that resisted microfissuring were devoid of the continuous sheets of carbides and/or extensive fine carbide precipitation. The microstructure observed in the HAZ microfissures suggests grain boundary liquation and formation of low melting liquid films enriched in niobium and carbon. The liquid originates primarily from the constitutional liquation of primary MC carbides, MNP phosphides, and fine MC carbides already present on the grain boundaries of the base metal. The solidification pattern of the liquid films on the microfissures is observed to follow a similar pattern as that of the fusion zone. The observation of microfissuring on boundaries which show continuous and/or semicontinuous sheets of resolidified structure suggests that HAZ microfissuring occurs due to the presence of low melting liquid films. The existence of continuous and/or semicontinuous liquid films and the added presence of phosphorus in them appear to be one of the major causes for extensive HAZ microfissuring in thermomechanically processed INCOLOY 903.     

析出相对Monel K-500合金冲击韧性的影响

通过一系列实验研究了Monel K-500合金的冲击韧性。结果表明,合金经550~650℃时效后其冲击断口呈沿晶形貌;在750~850℃时效时,其冲击韧性与强度呈正相关关系。根据对合金在不同热处理状态的析出相形态及分布的研究,揭示了形成这些现象的原因。合金在550~650℃时效时,在晶内析出的γ’相呈球状均匀分布,而在部分晶界附近的γ’相呈条棒状或排成帘状垂直于晶界分布,由此导致时效态合金在断裂时,裂纹沿晶界扩展。在750~850℃时效会导致合金形成大量沿晶界网状分布的二次MC相,从而降低合金的冲击韧性。     

Grain boundary γ″ precipitation and niobium segregation in inconel 718

The grain boundary γ″ precipitates in a commercial Inconel 718 have been critically examined by TEM. The results show that the grain boundaries were almost fully covered with γ″ particles which can account for the previous XPS finding of grain boundary enrichment in niobium for this alloy. These grain boundary γ″ precipitates appear to be disc-shaped, lie on the boundary plane, and have no habit-plane relationship with either of the neighboring grains. This finding suggests that the γ″ precipitates formed as a result of niobium segregation at the grain boundaries, rather than having the grain boundaries acting simply as the nucleation sites for preferential precipitation.     

气体雾化快凝W9高速钢粉末的组织特征

研究了颗粒粒度不同的气体雾化W9Mo3Cr4V高速钢粉末的组织、形貌及结构.结果表明:粉末由铁素体和奥氏体基体和分布在周围的MC及M2C型碳化物组成,基体组织为等轴晶及树枝晶,碳化物在空间上呈连续网状或树枝状分布;粉末中相的含量与粉末粒度相关,随高速钢粉末粒度减小,组织中的铁素体和MC型碳化物含量增加,奥氏体和M2C型碳化物含量减少.     

Nimonic 80A合金螺栓的组织织构及高温应力松弛行为

利用SEM与EBSD技术研究Nimonic 80A高温合金螺栓的组织织构特点,并对不同温度下的高温应力松弛行为及组织织构演变进行分析。结果表明,合金中γ相组织未形成显著织构,晶粒取向择尤情况与晶粒尺寸无对应性。合金中第二相主要为γ′相与Cr的碳化物,γ′相在基体中弥散分布,而Cr的碳化物分别在晶界析出和沿螺栓轴向“链状”分布,其分布特征与γ晶粒组织及取向无显著关联性。应力松弛前后,晶粒组织、碳化物分布及织构均无明显变化,但γ′相发生了一定的粗化。载荷一定时,温度对应力松弛行为存在显著影响,即较高温度下样品的应力松弛率较高。较高温度下位错滑移更易开动,与样品中更多晶粒表现出较高晶粒取向散布(GOS)值相对应,但各晶粒GOS值的高低未表现出晶粒取向与晶粒尺寸依赖性。     

Globular Structure of M2 High Speed Steel by Thermomechanical Treatment in the Semisolid State

The globular structure of M2 high speed steel in the rolled ‐ annealed and as cast conditions was investigated in the semisolid state. Metallographic observations resulted in globular austenite particles that were surrounded by a liquid phase. Dissolution of various carbides in the austenite phase at semisolid temperatures led to grain boundary liquation and formation of near‐spherical solid grains in a liquid matrix. Therefore, at the semisolid state, the solid particles were free from carbides. MC‐ type and M₆C‐ type eutectic carbides re‐ precipitated at the grain boundaries during cooling of the samples from the semisolid temperature. The variation of shape factor versus holding time and holding temperature was examined. A transition value for shape factor changes in high speed steels was achieved. The growth rate constants of the Ostwald ripening and the coalescence mechanisms were calculated by using the experimentally determined rate constant. It was observed that less liquid droplets were enclosed inside the solid particles compared with non‐ferrous alloys. Besides, it has been shown that at high solid fraction, the Ostwald ripening mechanism plays a prominent role in the coarsening phenomenon in comparison with the coalescence mechanism. Grains can rotate and arrange low misorientation with each other at high liquid contents, therefore low energetic grain boundaries form between these grains. These grain boundaries play an important role in the coalescence mechanism.     

Nimonic 80A合金螺栓的组织织构及高温应力松弛行为

利用SEM与EBSD技术研究Nimonic 80A高温合金螺栓的组织织构特点,并对不同温度下的高温应力松弛行为及组织织构演变进行分析。结果表明,合金中γ相组织未形成显著织构,晶粒取向择尤情况与晶粒尺寸无对应性。合金中第二相主要为γ′相与Cr的碳化物,γ′相在基体中弥散分布,而Cr的碳化物分别在晶界析出和沿螺栓轴向“链状”分布,其分布特征与γ晶粒组织及取向无显著关联性。应力松弛前后,晶粒组织、碳化物分布及织构均无明显变化,但γ′相发生了一定的粗化。载荷一定时,温度对应力松弛行为存在显著影响,即较高温度下样品的应力松弛率较高。较高温度下位错滑移更易开动,与样品中更多晶粒表现出较高晶粒取向散布(GOS)值相对应,但各晶粒GOS值的高低未表现出晶粒取向与晶粒尺寸依赖性。     

An AEM investigation of the formation of precipitate-free zones in an AI-16 Wt Pct Ag alloy: Determination of equilibrium and metastable solvus lines

Precipitation of the equilibrium y-phase at grain boundaries in an aged Al-16 wt pct (～4.5 at. pct) Ag alloy is responsible for the formation of a solute depleted region, free of metastable Guinier-Preston (GP) zones, in the immediate vicinity of the grain boundary. Solute concentration profiles have been obtained across these grain boundary regions using Analytical Electron Microscopy (AEM) in thin foils of the alloy aged at low temperatures. The Ag concentrations at the grain boundary (between γ precipitates) and at the edge of the precipitate-free zone have been used to determine the solid solubility of Ag in Al (the α/(α + γ) solvus) and the metastable GP zone solvus line, respectively.     

C元素对FGH96粉末高温合金显微组织和力学性能的影响

对C质量分数分别为0.05%和0.09%的FGH96合金进行了显微组织和力学性能的分析。结果发现:C元素含量较高时,除了碳化物数量明显增多外,还会在晶界处形成较大尺寸的块状MC碳化物;但是,C元素含量并未对原始颗粒边界(prior particle boundary,PPB)、晶粒度及γ′相产生明显的影响。C元素含量较高会提高FGH96合金在650℃时的抗拉强度和屈服强度,但会降低其塑性。在低周疲劳试验中,C元素含量较高,形成的大块MC型碳化物分布于表面或亚表面,将会作为裂纹起源从而显著降低合金的低周疲劳性能。     

The influence of solidification mode on heat affected zone microfissuring in a nickel-iron base superalloy

The heat affected zone (HAZ) microfissuring of thermomechanically processed Incology 903 with a duplex grain structure, has been examined with a view to understand the mechanism(s) of, and to reduce the incidence of microfissuring. Extensive formation of liquid films on the HAZ grain boundaries primarily due to the complete constitutional liquation of preexisting MNP phosphides, MC carbides and partial constitutional liquation of primary MX carbide insolubles was observed. The liquid films resulted in considerable microfissuring on the long warm worked grain boundaries and extensive grain boundary liquid film migration (LFM) on the fine recrystallized grain boundaries. The liquid films formed on the warm worked boundaries were observed to have undergone normal solidification accompanied with the formation of dendritic gamma and terminal interdendritic constituents. The exclusive occurrence of LFM only on the fine grains and not on warm worked grains is attributed to the increased driving force and velocity for LFM arising due to substantial interface curvature of the fine grains. It is shown that HAZ microfissuring is minimized if the liquid films on the HAZ grain boundaries can partially equilibrate by LFM instead of by normal solidification.