Microstructure and mechanical properties of nickel-based superalloy fabricated by laser powder-bed fusion using recycled powders

Evaluating the recyclability of powders in additive manufacturing has been a long-term challenge.In this study,the microstructure and mechanical properties of a nickel-based superalloy fabricated by laser powder-bed fusion(LPBF)using recycled powders were investigated.Re-melted powder surfaces,satellite particles,and deformed powders were found in the recycled powders,combined with a high-oxygencontent surface layer.The increasing oxygen content led to the formation of high-density oxide inclusions;moreover,printing-induced cracks widely occurred and mainly formed along the grain boundaries in the as-built LPBF nickel-based superalloys fabricated using recycled powders.A little change in the Si or Mn content did not increase the hot cracking susceptibility(HCS)of the printed parts.The changing aspect ratio and the surface damage of the recycled powders might contribute to increasing the crack density.Moreover,the configuration of cracks in the as-built parts led to anisotropic mechanical properties,mainly resulting in extremely low ductility vertical to the building direction,and the cracks mainly propagated along the cellular boundary owing to the existence of a brittle precipitation phase.

Hot working characteristics of HEXed PM nickel-based superalloy during hot compression

To study the hot deformation behavior of a new powder metallurgy nickel-based superalloy,hot compression tests were conducted in the temperature range of 1020−1110℃ with the strain rates of 0.001−1 s^−1.It is found that the flow stress of the superalloy decreases with increasing temperature and decreasing strain rate.An accurate constitutive equation is established using a hyperbolic-sine type expression.Moreover,processing map of the alloy is constructed to optimize its hot forging parameters.Three domains of dynamic recrystallization stability and instability regions are identified from the processing map at a strain of 0.7,respectively.The adiabatic shear band,intergranular crack and a combination of intergranular crack and wedge crack are demonstrated to be responsible for the instabilities.Comprehensively analyzing the processing map and microstructure,the optimal isothermal forging conditions for the superalloy is determined to be t=1075−1105℃ andε&=10^−3−10−2.8 s^−1.

Surface characteristics of rapidly solidified nickel-based superalloy pow-ders prepared by PREP

The surface microstructure and the surface segregation of FGH 95 nickel-basedsuperalloy powders prepared through plasma rotating electrode processing (PREP) have beeninvestigated by using SEM and AES. The results indicate that the surface microstructure of powderschanges from dendrite into cellular stricture as the particle size of powders decrease, and thepredominant precipitates solidified on the particle surfaces were identified as MC' type carbidesenriched with Nb and Ti. It was also indicated that along with the depth of particle surfaces, thesegregation layer of S, C and O elements are thick, and that of Ti, Cr elements are thin for largesire powders while they are in reverse for median size particles.

Effect of cooling rate on microstructure and tensile properties of powder metallurgy Ni-based superalloy

The effects of size distribution,morphology and volume fraction ofγ′phase and grain size on tensile properties of powder processed Ni-based superalloy were investigated by using two different quenching methods.Oil quenching and air cooling were adopted with cooling rate of 183°C/s and 4?15°C/s,respectively.The experimental results show that the average size of the secondaryγ′after oil quenching is 24.5 nm compared with 49.8 nm under air cooling,and corresponding volume fractions ofγ′are 29%and 34%,respectively.Meanwhile,the average grain size remains nearly equivalent from both oil-quenching and air-cooling specimens.The tensile strength at room temperature is higher for the oil-quenched specimen than the equivalent from the air-cooled specimen,but the difference approaches each other as the temperature increases to 650°C.The fractography clearly demonstrates that transgranular fracture governs the failure process at ambient temperature,in contrast to the intergranular fracture at 650°C or even higher temperature.These two mechanical responses indicate the strengthening effects ofγ′precipitates and grain boundary for polycrystalline Ni-based superalloys at different temperatures.

THE ROLE OF NIOBIUM IN NICKEL-BASED SUPERALLOYS AND CHARACTERIZATION OF PM ALLOY EP741NP

The role of niobium in nickel-based superalloys is reviewed. The importance of niobium as a strengthener is discussed. New developments in nickel-based superalloys are also briefly mentioned, including some results that show improved resistance to sulfidation by niobium. Research results from a current program on the role of niobium in the Russian powder metallurgy alloy EP741NP are presented. Future research plans on the role of niobium in superalloys are also discussed.

PARTICLE BOUNDARIES AND FRACTURE OF A POWDER METALLURGY SUPERALLOY

Nature of PPB precipitation of P/M Rene'95 and its effects on mechanical properties,frac- ture morphology and microfracture characteristics are discussed.Dense PPB precipitates make the boundaries brittle and lower the plasticity of the alloy.Fracture path is along the boundaries of particles.As PPB parameter increases,the interfaces between particles are strengthened.The fracture mode is changed from interparticle to transparticle.As a result,the plasticity at high temperatures and stress rupture life of the alloy are improved.

Spray forming and mechanical properties of a new type powder metallurgy superalloy

The deposited billet of a new type powder metallurgy （PM） superalloy FGH4095M for use in turbine disk manufac- turing has been fabricated using spray forming technology. The metallurgical quality of the deposited billet was analyzed in terms of density, texture, and grain size. Comparative research was done on the microstructure and mechanical properties between the flat disk preform prepared with hot isostatic pressing （HIP） and the same alloy forgings prepared with HIP followed by isothermal forging （IF）. The results show that the density of the spray-formed and nitrogen-atomized deposit billet is above 99% of the theoretical density, indicating a compact structure. The grains are uniform and fine. The billet has weak texture with a random distribution in the spray deposition direction and perpendicular to the direction of deposition. A part of atomizing nitrogen exists in the preform in the form of carbonitride. Nitrogen-induced microporosity causes the density reduction of the preform. Compared with the process of HIP＋IF, the superalloy FGH4095M after HIP has better mechanical properties at both room temperature and high temperature. The sizes of the 7~ phase are finer in microstructure of the preform after HIP in comparison with the forgings after HIP＋IE This work shows that SF＋HIP is a viable processing route for FGH4095M as a turbine-disk material.

Cooling γ′ precipitation behavior and strengthening in powder metallurgy su-peralloy FGH4096

Two cooling schemes （continuous cooling and interrupted cooling tests） were applied to investigate the cooling γ precipitation behavior in powder metallurgy superalloy FGH4096. The effect of cooling rate on cooling γ precipitation and the development of γ precipitates during cooling process were involved in this study. The ultimate tensile strength （ErrS） of the specimens in various cooling circumstances was tested. The experiential equations were obtained between the average sizes of secondary and tertiary γ precipitates, the strength, and cooling rate. The results show that they are inversely correlated with the cooling rate as well as the grain boundary changes from serrated to straight, the shape of secondary γ precipitates changes from irregular cuboidal to spherical, while the formed tertiary γ precipitates are always spherical. The interrupted cooling tests show that the average size of secondary γ precipitates increases as a linear function of interrupt temperature for a fixed cooling rate of 24℃/min. The strength first decreases and then increases against interrupt temperature, which is fundamentally caused by the multistage nucleation of γ precipitates during cooling process.

SOLIDIFICATION MICROSTRUCTURE OF Ni-BASE SUPERALLOY POWDER

The solidification microstructure and phase composition of Ni-base superalloy FGH95 pow- der with different mesh size have been investigated.The structure transition was found from dendrite in major into cellular structure as the powder size reduces and the cooling rate in- creases.The predominant phase was identified as MC-type carbide,with different morphologies,which may be related to their composition and the condition of solidification.Minor phases,such as boride,Laves and primary γ' are also present as ac- companiments of the carbide.

Oxidation during the production of FGH4095 superalloy powders by electrode induction-melt inert gas atomization

Super-clean and super-spherical FGH4095 superalloy powder is produced by the ceramic-free electrode inductionmelt inert gas atomization（EIGA） technique.A continuous and steady-state liquid metal flow is achieved at high-frequency（350 k Hz） alternating current and high electric power（100 k W）.The superalloy is immersed in a high-frequency induction coil,and the liquid metal falling into a supersonic nozzle is atomized by an Ar gas of high kinetic gas energy.Numerical calculations are performed to optimize the structure parameters for the nozzle tip.The undesired oxidation reaction of alloying elements starts at 1000℃ with the reaction originating from the active sites on the powder surfaces,leading to the formation of oxides,MexOy.The role of active sites and kinetic factors associated with the diffusion of oxygen present in the atomization gas streams are also examined.The observed results reveal that the oxidation process occurring at the surface of the produced powders gradually moves toward the core,and that there exists a clear interface between the product layer and the reactant.The present study lays a theoretical foundation for controlling the oxidation of nickel-based superalloy powders from the powder process step.

CRITICAL ISSUES OF POWDER METALLURGY TURBINE DISKS

P/M superalloy disks obtain their final strength by appropriate heat treatments; the maximum attainable strength depends on the rapid cooling rate from the solution annealing. A rapid quench of a large disk forging can cause two problems, surface cracking and shape distortion.In the past,many attempts employ the finite element code to model and to predict temperature evolution and induced stress distribution in a large turbine disk. The major difficulty was the correct description of alloy behavior; particularly the thermomechanical properties and the failure criteria of material during the cooling. High temperature fatigue resistance is always the key requirement for disk materials. New methodology of residual life management emphasizes the initiation as well as the propagation of the cracks developed under the service conditions. One of major challenges to P/M superalloys is the time-dependent behavior of fatigue cracking, which relates to the well-known SAGBO (stress-assisted grain boundary oxidation) phenomenon.A great effort has been done to understand the micro-mechanism of time-dependent fatigue crack propagation resulted in the second generation of P/M superalloys. Further improvement on temperature capability of disk alloys at rim area may lead to the idea of dual-property disks.Different grain structures at different portions of a large disk are possible,as the property requirements for different locations are different. This goal is achievable if the thermal history at specific disk locations can be controlled to develop desirable microstructures and properties.Some suggestions on the future direction of research efforts will be discused.

Prediction on grinding force during grinding powder metallurgy nickel-based superalloy FGH96 with electroplated CBN abrasive wheel

In this article,a grinding force model,which is on the basis of cutting process of single abrasive grains combined with the method of theoretical derivation and empirical formula by analyzing the formation mechanism of grinding force,was established.Three key factors have been taken into accounts in this model,such as the contact friction force between abrasive grains and materials,the plastic deformation of material in the process of abrasive plowing,and the shear strain effect of material during the process of cutting chips formation.The model was finally validated by the orthogonal grinding experiment of powder metallurgy nickel-based superalloy FGH96 by using the electroplated CBN abrasive wheel.Grinding force values of prediction and experiment were in good consistency.The errors of tangential grinding force and normal grinding force were 9.8%and 13.6%,respectively.The contributions of sliding force,plowing force and chip formation force were also analyzed.In addition,the tangential forces of sliding,plowing and chip formation are 14%,19%and 11%of the normal forces on average,respectively.The pro-posed grinding forcemodel is not only in favor of optimizing the grinding parameters and improving grinding efficiency,but also contributes to study some other grinding subjects(e.g.abrasive wheel wear,grinding heat,residual stress).

An investigation on machined surface quality and tool wear during creep feed grinding of powder metallurgy nickel-based superalloy FGH96 with alumina abrasive wheels

In this study,the machined surface quality of powder metallurgy nickel-based superalloy FGH96(similar to Rene88DT)and the grinding characteristics of brown alumina(BA)and microcrystalline alumina(MA)abrasive wheels were comparatively analyzed during creep feed grinding.The infuences of the grinding parameters(abrasive wheel speed,workpiece infeed speed,and depth of cut)on the grinding force,grinding temperature,surface roughness,surface morphology,tool wear,and grinding ratio were analyzed comprehensively.The experimental results showed that there was no significant difference in terms of the machined surface quality and grinding characteristics of FGH96 during grinding with the two types of abrasive wheels.This was mainly because the grinding advantages of the MA wheel were weakened for the difficult-to-cut FGH96 material.Moreover,both the BA and MA abrasive wheeIs exhibited severe tool wear in the form of wheel clogging and workpiece material adhesion.Finally,an analytical model for prediction of the grinding ratio was established by combining the tool wear volume,grinding force,and grinding length.The acceptable errors between the predicted and experimental grinding ratios(ranging from 0.6 to 1.8)were 7.56%and 6.31%for the BA and MA abrasive wheels,respectively.This model can be used to evaluate quantitatively the grinding performance of an alumina abrasive wheel,and is therefore helpful for optimizing the grinding parameters in the creep feed grinding process.

Evolution of grain size and grain shape during thermomechanical processing in a powder metallurgical nickel-based superalloy

With a strain rate range of 0.01–10 s^(−1) and a deformation temperature range of 1110–1200℃,the isothermal compression test was performed on one powder metallurgy superalloy which is macroscopic segregation free.Using electron backscatter diffraction,the effect of strain rate and deformation temperature on grain shape and grain size of superalloys during thermal deformation was studied.The results established that exquisite and equiaxed dynamic recrystallization(DRX)grains are procured at supernal deformation temperature and high strain rate because of the high dislocation density.At the same time,the interaction between high DRX nucleation rate and low grain growth rate at high strain rate is favorable in making finer DRX grains.The equivalent medial grain size expanded with lowering strain rate and elevating proof temperature.Moreover,the grain shape was researched by the effective method of aspect ratio.Most aspect ratio of original grains is 0.61,and the aspect ratio has important implications for DRX and grain growth process.The average aspect ratio increases slightly when deformation temperature rises from 1110 to 1140℃,while the average aspect ratio increases memorably as the deformation temperature is higher than 1140℃.

航空发动机应用领域粉末高温合金的研究进展

【目的】总结粉末高温合金的材料设计和制备工艺等方面的研究进展,为研究延长航空发动机涡轮盘等关键部件的使用寿命打下基础。【研究现状】针对近年来国内外航空发动机涡轮盘等关键部件主要材料的粉末高温合金,综述多种类型的粉末高温合金的元素组成及制备工艺,概括碳、钽、铪、硼、锆、钴、钛、稀土元素等微量元素对粉末高温合金性能的影响,总结热等静压、热挤压、粉末注射成型、增材制造等制备工艺对粉末高温合金性能的影响。【结论与展望】在材料设计方面,应优化粉末高温合金元素组成,探索添加更多高性能元素,制备更耐高温、耐氧化、力学性能优异、服役寿命长的粉末高温合金;在制备工艺方面,优化热等静压及热挤压工艺参数,继续探索完善粉末注射成型、增材制造工艺。

Influence of Post-Treatment Process on Microstructure and Properties of Laser Additively Manufactured Nickel-Based Superalloy

Defects such as cracks and micropores exist in nickel-based superalloy during laser powder bed fusion(LPBF),hindering their application in various fields.Hot isostatic pressing(HIP)was combined with conventional heat treatment(HT)to obtain LPBF nickel-based superalloy parts with ideal properties and fewer defects.The results show that HIP process can improve the densification,while the conventional HT can eliminate the micro-defects to improve the mechanical properties.After HIP treatment,the defect volume fraction of LPBF specimens decreases.After HT,the defect content of HIP+HT specimens increases slightly.After post-treatment,the hardness shows a decreasing trend,and the tensile strength and post-break elongation of HIP+HT specimens increase to 1326 MPa and 21.3%,respectively,at room temperature.

Microstructure and microtexture evolution characteristics of a powder metallurgy Ni-based superalloy during static recrystallization

Static recrystallization(SRX)characteristics of a powder metallurgy superalloy were investigated by isothermal compression at 1080–1170℃ under strain rates of 0.01–0.1 s^(−1),strains of 0.1,0.22,or 0.5,and holding time of 0–300 s.The impacts of temperature,strain rate,holding time,and strain on the SRXed grain size,volume fraction,and microtexture were explored by electron backscatter diffraction technique.It was found that temperature played a key role in these processes.As SRX progressed,the<110>fiber parallel to the axis compression direction gradually weakened and was replaced by the<001>fiber because<001>was the preferred recrystallization orientation and grain growth direction for the Ni-based superalloy.Moreover,high temperatures and low strain rates promoted the formation of the<001>fiber.Three nucleation mechanisms during SRX process were found:grain boundary bulging,primary twin assistance,and subgrain coalescence.Grain boundary bulging occurred under all process conditions;however,at low temperatures and high strain rates,the latter two mechanisms could provide additional nucleation modes.In addition,SRX size and volume fraction models were established.

Precipitation behavior of γ′ phase in superalloy FGH96 under interrupted cooling test

The precipitation behavior of γ′ phase,under various interrupt cooling tests after 1170℃,solution treatment was examined.The results indicate that the size of secondary γ′ precipitates increases with the decrease of interrupt temperature,and the shape changes from spherical to butterfly like.The fine tertiary γ′ can form either during the post cool air quenching at high interrupt-temperatures,or during the specified 5℃ min-1cooling.Air quenching at high temperatures cannot suppress further nucleation of tertiary γ′ phase.

Effect of solution cooling rate on the γ′ precipitation behaviors of a Ni-base P/M superalloy

The effect of cooling rate on the cooling γ′ precipitation behaviors was investigated in a Ni-base powder/metallurgy （P/M） superalloy （FGH4096）. The empirical equations were established between the cooling rate and the average sizes of secondary and tertiary γ′ precipitates within grains and tertiary γ′ precipitates at grain boundaries, as well as the apparent width of grain boundaries. The results show that the average sizes of secondary or tertiary γ′ precipitates are inversely correlated with the cooling rate. The shape of secondary γ′ precipitates within grains changes from butterfly-like to spherical with the increase of cooling rate, but all the tertiaryγ′ precipitates formed are spherical in shape. It is also found that tertiary γ′ may be precipitated in the latter part of the cooling cycle only if the cooling rate is not faster than 4.3℃/s, and the apparent width of grain boundaries decreases linearly with the increase of cooling rate.

Effect of oxygen content and heat treatment on carbide precipitation behavior in PM Ni-base superalloys

The influence of oxygen content and heat treatment on the evolution of carbides in a powder metallurgy （PM） Ni-base superalloy was characterized. The results reveal that oxygen content has little influence on the precipitation of carbides inside the particles. However, under the consolidated state, stable Ti oxides on the particle surface act as nuclei for the precipitation of prior particle boundaries （PPB）. Also, oxygen can diffuse internally along grain boundaries under compressive stress, which favors the precipitation of carbides inside the particles. Therefore, a higher amount of carbides will appear with more oxygen content in the case of consolidated alloys. It is also observed that PPB can be disrupted into discontinuous particles at 1200℃, but this carbide network is hard to be eliminated completely. The combined MC-M23C6 morphology approves the nucleation and growth mechanism of carbide evolution.