Nickel-based Superalloy CMSX-4 Research Articles

Effects of surface hardening by laser shock peening and shot peening on a nickel-based single-crystal superalloy CMSX-4

Improving the expected life of nickel-based single-crystal superalloy turbine components by surface hardening treatments including laser shock peening (LSP) and mechanical shot peening (MSP) are of particular interest for mitigation of life limiting damage such as environmental assisted cracking in hot section components of gas turbines. In the present study the effects of LSP and MSP on the surface roughness, microhardness and work hardening of a nickel-based single crystal superalloy CMSX-4® have been assessed. Surface roughness was measured using laser profilometry. The degree of work hardening was measured using electron backscattered diffraction with local misorientation analysis. The analysis showed evidence for a work hardening layer in the MSP sample to a depth of approximately 70 μm. Sets of slip bands extending far into the bulk of the sample were observed in the LSP-treated sample, without any evidence of a work hardening layer. Microhardness measurements used to gauge the depth of residual stress showed that LSP produced a much deeper hardness profile than MSP, with compressive residual stress depths of 1000 μm and 200 μm in LSP and MSP respectively. The retention of hardness after a heat treatment of 50 h at 700 °C was more prominent in the LSP sample than in the MSP sample. LSP and MSP have therefore been shown to be at the opposite ends of the spectrum of surface hardening treatments of CMSX-4, with LSP giving milder hardening, but to a greater depth.

An insight into the creep failure mechanism of sliver defect in the second-generation nickel-based single crystal superalloy CMSX-4

Sliver defects are common casting imperfections in the preparation of single crystal blades, significantly impacting the high-temperature mechanical performance of blades and potentially leading to blade failure. A detailed study was conducted on the microstructure of sliver in the second-generation nickel-based single crystal superalloy CMSX-4, focusing on its influence on creep performance at 980 °C/250 MPa. Results indicate a substantial impact of sliver on the creep performance of single crystal superalloys, with a 26.37 % reduction in creep rupture time for samples with sliver compared to those without. Fracture analysis reveals that sliver primarily contributes to performance deterioration by promoting the extension of grain boundary microcracks through grain boundary sliding during the creep process, accelerating sample fracture. Utilizing crystal plasticity theory, a successful fit was achieved for the creep rupture life of samples with sliver, allowing the prediction of fracture life for samples with different orientations of slivers. Predictive results suggest that, for CMSX-4 alloy, the orientation of the sliver should be restricted to within 8°.

New insights into the optimisation of the solution heat treatment process and properties of CMSX-4 superalloys

For nickel-based single-crystal superalloys, simultaneously reducing the segregation and optimising the microstructure is a primary challenge in the field of heat treatment. To further improve rupture life, the element partition, microstructure evolution, and creep behaviour of the second-generation nickel-based single-crystal superalloy CMSX-4 under five different solution processes were studied using electron microprobe, scanning electron microscopy, and transmission electron microscopy. Under the same conditions, both continuous heating and remelting heat treatment exhibited higher elements homogenisation efficiency. Moreover, it was found that the improvement of element segregation can make γ′ phase smaller and more uniform. These heat treatments reduced the incipient melting tendency or eliminated the incipient melting eutectic, thereby increasing the peak heat treatment temperature of the CMSX-4 alloy. However, remelting heat treatment results in a significant increase in the porosity of the alloy, leading to a deterioration in performance. Finally, based on the above study, a novel process combining stepwise heating and continuous heating was proposed, which not only increased the peak solid-solution temperature but also prevented the incipient melting and optimized the microstructure. After using the novel process, the durability of the alloy increased by 48 % from 240 to 356 h under the test conditions of 980 °C/250 MPa. The higher proportion of the γ′ phase, narrower matrix channel, and denser dislocation network were the main reasons for the improvement in the rupture life.

Comparison of Isothermal and Adiabatic Elasticity Characteristics of the Single Crystal Nickel-Based Superalloy CMSX-4 in the Temperature Range Between Room Temperature and 1300°C

Based on the results of performed thermophysical measurements and available experimental data for adiabatic elastic stiffnesses, isothermal elastic characteristics of the single crystal nickel-based superalloy CMSX-4 have been calculated for a wide temperature range, from room temperature to 1300°C. According to the results obtained, the adiabatic and isothermal values of such elastic characteristics as elastic stiffnesses {{c}_{{11}}}, {{c}_{{12}}} and bulk modulus of elasticity B differ significantly at high temperatures. The reasons for this are significant changes in the thermophysical properties of the alloy with temperature and a temperature increase of its Poisson’s ratio approaching the limiting value for cubic crystals, equal to 0.5. It is shown that the use of adiabatic elastic constants instead of isothermal ones in engineering calculations affects the relationship between the volumetric strain and hydrostatic stress, and this effect is similar to introducing a field of thermal dilatation into the analyzed object. At low temperatures, this effect is small, but at high temperatures, typical for the service conditions of the blade material of aircraft gas turbine engines, it increases many times.

A Crystallographic Basis for Critically Evaluating the Mechanisms for Secondary Grain Formation During Directional Solidification

AbstractA crystallography-based method is presented for the critical appraisal of possible mechanisms that trigger the formation of secondary grains during directional solidification. The method permits an analysis of a large population of defects, while avoiding the pitfalls of the metallographic sectioning approach that is affected by dendrite stereology. Here, the nickel-base superalloy CMSX-4, an alloy commonly used for single crystal turbine blade applications, is studied. All secondary grains originate exclusively at the external surface and when the off-axial primary $$\langle 0\,0\,1\rangle$$ ⟨ 0 0 1 ⟩ crystal orientations are measured, are evident at both the converging and diverging dispositions of the single crystal primary dendrites without a noticeable bias. Almost all of the secondary grains have low misorientations, with an average misorientation between 5 to 15 deg. No systematic deviation between the individual $$\langle 0\,0\,1\rangle$$ ⟨ 0 0 1 ⟩ orientations of the secondary grain and the single crystal is observed. A significant twist contribution about an axis within ~ 30 deg from one of the secondary arms occurs when primary arms converge on the external surface, but both twist and tilt prevail for the diverging case. Both nucleation and buoyancy driven thermo-solutal convection can be eliminated as potential mechanisms. Thermo-mechanical deformation is deduced to be the most likely mechanism; deformation must originate in the vicinity of the primary dendrite tips. It is proposed that dendrite deflection arises primarily from the resistance encountered by the primary tips with the external surface during axial contraction in the presence of a dominant vertical thermal gradient.

Development of mullite-alumina ceramic shells for precision investment casting of single-crystal high-pressure turbine blades

Alumina-mullite ceramic shell moulds were developed to cast single-crystal hollow high-pressure turbine blades (SX-HPTB). Mullite and fine alumina powders were used as fillers. Two colloidal silica binders were used to bind the filler particles. One colloidal silica binder (binder A) had no polymer and the second colloidal silica binder (binder B) had 8 wt % polymer. Eight slurry compositions with fine alumina substitution (0, 10, 30 and 50 wt %) were prepared. Silica cores were used to achieve hollow castings. The effect of alumina substitution and binders on the slurry characteristics, flexural strength of green and fired samples, air permeability and self-load sag resistance was studied. It was observed that with an increase in alumina percentage, the test specimens showed increased viscosity, pick-up weight, density, green strength and fired residual strength. In addition, the slurries prepared from binder B possessed larger values of viscosity and pick-up weight compared to the slurries prepared from binder A. The residual strength of fired test specimens containing binder A was higher than those containing binder B. The test specimens with 30 wt % fine alumina substitution showed the highest self-load sag resistance w.r.t. each test temperature. Also, the air permeability of the fired samples was higher than the green (de-waxed) samples. The casting of hollow HPTB components was performed at two temperatures (1525 °C and 1550 °C) using nickel-based superalloy CMSX4. The HPTB components, cast at 1550 oC from ceramic shell mould having binder B and 30 wt % fine alumina substitution, resulted in an acceptable aerofoil profile and surface roughness.

Revealing dynamic processes in laser powder bed fusion with in situ X-ray diffraction at PETRA III.

The high flux combined with the high energy of the monochromatic synchrotron radiation available at modern synchrotron facilities offers vast possibilities for fundamental research on metal processing technologies. Especially in the case of laser powder bed fusion (LPBF), an additive manufacturing technology for the manufacturing of complex-shaped metallic parts, in situ methods are necessary to understand the highly dynamic thermal, mechanical, and metallurgical processes involved in the creation of the parts. At PETRA III, Deutsches Elektronen-Synchrotron, a customized LPBF system featuring all essential functions of an industrial LPBF system, is used for in situ x-ray diffraction research. Three use cases with different experimental setups and research questions are presented to demonstrate research opportunities. First, the influence of substrate pre-heating and a complex scan pattern on the strain and internal stress progression during the manufacturing of Inconel 625 parts is investigated. Second, a study on the nickel-base superalloy CMSX-4 reveals the formation and dissolution of γ' precipitates depending on the scan pattern in different part locations. Third, phase transitions during melting and solidification of an intermetallic γ-TiAl based alloy are examined, and the advantages of using thin platelet-shaped specimens to resolve the phase components are discussed. The presented cases give an overview of in situ x-ray diffraction experiments at PETRA III for research on the LPBF technology and provide information on specific experimental procedures.

Convective effects on columnar dendritic solidification – A multiscale dendritic needle network study

Gravity-induced buoyancy, inevitable in most solidification processes, substantially alters the dynamics of crystal growth, such that incorporating fluid flow in solidification models is crucial to understand and predict key aspects of microstructure selection. Here, we present a multi-scale Dendritic Needle Network (DNN) model for directional solidification that includes buoyant flow in the liquid, and apply it to a range of alloys and growth conditions. After a brief presentation of the model, we study the selection of stable primary dendrite arm spacings in Al-4at.%Cu and in Ti-45at.%Al alloys under different gravity levels, comparing both applications to published phase-field results and experimental measurements. Then, we simulate the oscillatory growth behavior recently reported via X-ray in situ imaging of directional solidification of nickel-based superalloy CMSX-4. In this last application, the DNN simulations manage to reproduce the oscillatory growth behavior, and hence permit identifying the fundamental mechanisms behind the oscillatory growth regime. In particular, we show that sustained oscillations occur when the average liquid flow velocity is close to the crystal growth velocity, and that primary dendritic spacings also play a crucial role in the oscillatory behavior.

Effect of Pre-creep Time on Creep Life of Nickel-based Single Crystal Superalloy CMSX-4

Abstract The effect of overheating with different time on creep life and strain curve of CMSX-4 nickel-based single crystal superalloy was studied. The overheating tests at different temperatures and stresses were carried out. The tests results showed that the duration of the second stage of creep would be reduced when the overheating happened at the beginning of the creep test. The deformation of the alloy quickly entered the third stage of creep, which obviously reduces the creep life and total strain of the material. When the overheating occurs in the second stage of creep, the rate of strain would increase after overheating and then the total creep life decreased. When the overheating was introduced at the beginning of the creep tests, the strain accumulation during the overheating was greater than that in the second stage of creep. However, the rate of strain after the overheating at the beginning is lower than that in the second stage of creep.

Deformation Modes in the Single-Crystal Nickel-Based Superalloy CMSX-4 During Compressive Deformation at 1000 °C

Deformation Modes in the Single-Crystal Nickel-Based Superalloy CMSX-4 During Compressive Deformation at 1000 °C

Study on Creep Damage of Ni-Based Superalloy Caused by Variable Load Conditions at Elevated Temperatures.

Higher fatigue and creep resistance at high temperatures are the essential properties for materials such as those used in gas turbines for power generation and aircraft turbines. Therefore, the nickel-based superalloy CMSX-4 was developed through single-crystal casting to satisfy these requirements. In this study, the CMSX-4 creep test results reported by previous researchers were used to mathematically derive an equation to estimate the amount of creep damage occurring under variable load conditions. In addition, low-cycle fatigue tests were performed, and the effect of creep damage occurring during fatigue on material failure was described.

Deep cold rolling of single crystal nickel-based superalloy CMSX-4

Nickel-based superalloys used in the aerospace industry are regularly subjected to high temperature and stress cycles. In order to extend component life, many components are subjected to a cold work process during manufacturing. One such technique is deep cold rolling, a highly controllable process which utilises a roller ball to impart cold work and deep compressive residual stress into a surface. In this study, local misorientation analysis of electron backscattered diffraction data has been used to quantify the surface cold worked layers in single crystal samples of the superalloy CMSX-4®, deep cold rolled with different pressures, ball diameters and roll orientations. As expected, it was found that greater pressure and ball diameter both increased the cold work depth, with pressure also affecting the amount of cold work per depth. Different roll orientations produced very similar distributions of cold work. In comparison with mechanical shot peening, another surface hardening technique, deep cold rolling is shown to produce a much deeper layer of relatively low cold work.

Assessment of thermo-mechanical fatigue in a nickel-based single-crystal superalloy CMSX-4 accounting for temperature gradient effects

Turbine blades are working under complex thermal gradient mechanical loading conditions. In the present study, a nickel-based single-crystal superalloy CMSX-4 is experimentally and computationally investigated under the thermo-mechanical fatigue (TMF) and thermal gradient mechanical fatigue (TGMF) loading conditions of the in-phase and out-of-phase thermal-mechanical angel. The fatigue life of TGMF with and without the thermal barrier coating was studied. It was confirmed that the lifetime of TGMF is affected by the temperature gradient significantly and substantially differs from conventional isothermal high temperature fatigue and thermo-mechanical fatigue. Since conventional fatigue models fail to characterize the TGMF, a modified model considers temperature gradient effects and thermal-mechanical phase angle and can describe the TGMF lifetime of the single-crystal superalloy reasonably.

Investigation of Elastic Properties of the Single-Crystal Nickel-Base Superalloy CMSX-4 in the Temperature Interval between Room Temperature and 1300 °C

The elastic properties of the single-crystal nickel-base superalloy CMSX-4 used as a blade material in gas turbines were investigated by the sonic resonance method in the temperature interval between room temperature and 1300 °C. Elastic constants at such high temperatures are needed to model the mechanical behavior of blade material during manufacturing (hot isostatic pressing) as well as during technical accidents which may happen in service (overheating). High reliability of the results was achieved using specimens of different crystallographic orientations, exciting various vibration modes as well as precise measurement of the material density and thermal expansion required for modeling the resonance frequencies by finite element method. Combining the results measured in this work and literature data the elastic constants of the γ- and γ′-phases were predicted. This prediction was supported by measurement of the temperature dependence of the γ′-fraction. All data obtained in this work are given in numerical or analytical forms and can be easily used for different scientific and engineering calculations.

Synchrotron 3D μ-Tomography of Porosity during Hot Isostatic Pressing of a Single-Crystal Nickel-Base Superalloy

The evolution of microporosity in single-crystal nickel-base superalloy CMSX-4 during hot isostatic pressing has been investigated by high resolution tomography at the European Synchrotron Radiation Facility in Grenoble. The kinetic dependencies of microporosity annihilation in the superalloy in initially as-cast and homogenized conditions were obtained. It was shown that smaller homogenization pores of about 5-10 μm in size are rapidly annihilate during hot isostatic pressing, while annihilation of larger solidification pores of size up to a few hundred micrometer takes a long time. After commercial hot isostatic pressing at 1288 °C, 103 MPa, 4 h only rare pores smaller than 20 μm remain, which are not critical for fatigue strength.

Thermal-solutal-fluid flow of channel segregation during directional solidification of single-crystal nickel-based superalloys

Channel segregation – known as freckle – is one of the most complex defects which severely limit mechanical properties of investment cast single-crystal turbine blades. The freckle phenomenon is induced by the thermal-solutal-fluid flow instability during solidification process; it is therefore important to gain better understanding of the fluid flow, heat transfer and species transport during the investment casting process. In this work, a three-dimensional Eulerian two-phase model is developed to investigate chimney behaviours and the evolution of channel segregation in the directional solidification of nickel-based single crystal superalloy CMSX-4. The results reveal that the channels are merely distributed on the surface of ingot backed up with targeted experiments, and the morphology of the predicted channel segregation is also consistent with the observed freckle chains. By ignoring lateral heat flux, deviation in the prediction of channel segregation using Rayleigh number criterion is anticipated, because not all the chimneys can be developed into channel segregation under the significant perturbation. In the mushy zone, the perturbation of the melt convection from the horizontal direction to the casting direction leads to the extinction of existing chimneys, thereby exacerbating channel segregation. Once the stable channel segregation is formed, it will be developed steadily under further solute enrichment caused by thermal-solutal convection. Channel segregations is difficult to develop continuously in the centre of the representative rod, while channels near the lateral walls are more likely to develop stable flow along the casting direction. It is suggested that the weaker lateral heat flux can suppress the formation of channel segregation, providing an effective process design criterion for the freckle mitigation during the single crystal casting.

Enhanced creep properties of nickel-base single crystal superalloy CMSX-4 by high magnetic field

Abstract The creep properties of nickel-base single crystal superalloy CMSX-4 with and without high magnetic field at 980 °C/250 MPa are investigated. Superalloy CMSX-4 is shown with an excellent rupture life under high magnetic field. Fracture surface results indicate that small square-shaped facets are shown and microporosities are formed at the bottom of dimple without high magnetic field, while the dimple surface shows large square-shaped facets and microporosities disappear from the bottom of dimple with high magnetic field. The mechanism of the enhancement of rupture life and the change of fracture behavior are explored in detail.

Refinement and Experimental Validation of a Vacancy Model of Pore Annihilation in Single-Crystal Nickel-Base Superalloys During Hot Isostatic Pressing

Initially as-cast and homogenized single-crystals of nickel-base superalloy CMSX-4 were subjected to hot isostatic pressing at temperature of 1288 °C. Two series of experiments were performed: under the same pressure of 103 MPa but with different durations, between 0.5 and 6 h, and under different pressures, between 15 and 150 MPa, but for the same time of 0.5 h. The porosity annihilation was investigated metallographically and by high resolution synchrotron X-ray tomography. The obtained experimental results were compared with the predictions of the vacancy model proposed recently in our group. In this work the model was further refined by coupling with X-ray tomography. The model describes the evolution of the pore arrays enclosed in the 3D synchrotron tomograms during hot isostatic pressing and properly predicts the time and stress dependences of the pore annihilation kinetics. The validated model and the obtained experimental results can be used for selecting the optimal technological parameters such as applied pressure and processing time.

Three-dimensional analysis of dendrites via automated serial sectioning using a Robo-Met.3D

The dendrite morphologies of the cast nickel-based superalloy CMSX-4® (CMSX-4® is registered trademarks of the Cannon-Muskegon Corporation) and the austenitic stainless steel HP microalloy have been obtained via an automated serial-sectioning process which allows three-dimensional (3D) microstructural characterization. The dendrite arm spacing, volume fraction of segregation, and fraction of porosity have been determined. This technique not only increases the depth, scope, and level of detailed microstructural characterization but also delivers microstructural data for modeling and simulation.

Some new observations on interface reaction between nickel-based single crystal superalloy CMSX-4 and silicon oxide ceramic core

To clarify and comprehend the interfacial compatibility of single crystal superalloy and ceramic core, the interface reaction of nickel-based single crystal superalloy CMSX-4 and silicon oxide ceramic core during directional solidification is investigated. The results revealed that a continuously distributed Al2O3 layer is formed at the interface of superalloy / silicon oxide ceramic core. Moreover, it is also found that a discontinuously distributed Ta/Ti enrichment carbide layer, (Ta/Ti)C, is formed at the interface of Al2O3 layer/superalloy. The formation mechanism of interface reaction between the nickel-based single crystal superalloy and silicon oxide ceramic core is analyzed.