Ru对镍基单晶热暴露组织演变及持久性能的影响

对比研究了不含Ru的USTB-F7及添加2.5 wt％ Ru的USTB-F8两种镍基单晶高温合金的组织稳定性和持久性能.标准热处理与1100℃长期热暴露组织研究表明:合金USTB-F7中γ′相形貌介于球形和立方形之间,属中间态形貌;热暴露2000 h后,其形貌仍保持稳定,仅发生粗化而未发生筏排化.Ru的添加使Re元素在γ/γ′中的分配比增大,提高了合金USTB-F8的γ/γ′点阵错配度和γ'相的立方度,从而加速了长期热暴露过程中的筏排化进程,经2000 h热暴露发生了明显的筏排化现象.同时,合金USTB-F7热暴露700 h后在枝晶干处析出了富集Re、W和Cr元素的TCP相,Ru的加入有效地抑制了TCP相的析出,合金USTB-F8直至2000 h仍未析出TCP相.1100℃/140MPa持久性能测试表明,Ru显著提高合金的持久寿命,这与Ru增加合金中的y相体积分数和γ/γ′点阵错配度,促进筏排组织的形成,并减小时效组织中的γ通道宽度有关.     

Lattice-parameter misfits between the γ and γ′ phases in single crystals of nickel superalloys

X-ray diffractometry has been used to study the transformation of the profiles of X-ray diffraction lines (222), (004), (003) and to determine the values of the lattice misfit between the γ and γ′ phases (γ/γ′ misfit) for single crystals of nickel superalloys ZhS6U, ZhS30, ZhS32, VZhM1, and VZhM4 in the as-cast state and after heat treatment. It has been established that with an increase in the γ/γ′ misfit there increase tetragonal distortions of the fcc lattice of the γ solid solution. For the single crystals of VZhM4 alloyed with rhenium and ruthenium, splitting of the superlattice reflection of the strengthening γ′ phase has been revealed. The structural regularities revealed testify to qualitative changes in the factors that govern the redistribution of refractory alloying elements between the lattices of the γ and γ′ phases, for example, of Mo in the presence of Re and Ru.     

Lattice misfit during ageing of a polycrystalline nickel-base superalloy

The temporal evolution of the lattice parameters and lattice misfit of an advanced polycrystalline nickel-base superalloy have been studied in situ during an ageing heat treatment using synchrotron X-ray diffraction. During ageing, the γ and γ′ lattice parameters were both observed to decrease, a trend that cannot be attributed to a loss of coherency alone. Phase-extracted γ′ replicated this behaviour. Atom probe tomography was used to measure the compositional changes between the start and end of the ageing heat treatment. Using these data, a thermodynamic assessment was made using the software ThermoCalc of the structural change across the interface between γ and γ′. Subsequently, the unconstrained lattice parameters were estimated and were shown to be in good agreement with the X-ray diffraction measurements. Thus, the observed anomalous lattice misfit behaviour was concluded to be dominated by elemental exchange between the γ and γ′ phases during ageing.     

Microstructures of Rene 142 nickel-based superalloy fabricated by electron beam melting

Rene 142, a commercial, columnar grained, gas turbine airfoil Ni-based superalloy, has been fabricated from a pre-alloyed, atomized powder by additive manufacturing using electron beam melting. Monolithic components having [0 0 1] oriented, columnar grain structures exhibited a creep-optimized 59% volume fraction of cuboidal, coherent, γ′-phase precipitates averaging 275 nm on the side, and with γ/γ′ channel widths ranging from 25 to 75 nm. Transmission electron microscopy, utilizing bright and dark field imaging of optimally oriented γ/γ′ interfaces showed prominent misfit coherency strains as δ-fringe patterns. Corresponding hardness measurements also indicated the possibility of creep strength comparable with the commercial alloy. The notable feature of this study was the monolithic development of desirable superalloy properties without conventional, multi-step heat treatments.     

A neutron diffraction study of lattice distortion,mismatch and misorientation in a single-crystal superalloy after different heat treatments

Two-dimensional neutron diffraction measurements of superlattice and fundamental lattice reflections from a single-crystal superalloy confirm the existence of angular distortion and shear stress in the γ′ phase, and reveal its correlation with the morphology and deformation of the γ′ phase during heat treatment. The tetragonal distortions with c/a > 1 are developed and retained during subsequent heat treatments, whereas the angular distortions are enhanced for the γ′ phase during the aging treatments. The evolution of the lattice mismatch and anisotropy during the subsequent heat treatments are consistent with the transformation of certain macroscopic anisotropic compositional and stress distributions in the as-cast sample to the microscopic level at the γ/γ′-interface upon reprecipitation and the growth of the γ′ from the supersaturated γ-matrix. The high negative γ/γ′ lattice mismatch of the alloy is consistent with the high levels of refractory elements, in particular Cr, in the alloy. Comparison between superlattice and fundamental lattice reflections is revealing. Firstly, the existence of lattice misorientation at the γ/γ′-interface and the discrete misorientations from the splitting of coherently aligned aggregates of γ′-precipitates on the smoothly distributed γ -matrix is shown. Secondly, the measured lattice misorientation correlates with the spacing of dislocations at the γ/γ′-interface and evidenced by the transmission electron microscopy observation. Furthermore, it indicates the anisotropic distribution of dendrites along crystal growth axis and the presence of small misoriented higher-order dendrite arms in variously heat-treated samples.     

Improved High-Temperature Microstructural Stability and Creep Property of Novel Co-Base Single-Crystal Alloys Containing Ta and Ti

The influence of Ta and Ti additions on microstructural stability and creep behavior in novel Co-Al-W base single-crystal alloys has been investigated. Compared to the ternary alloy, the γ′ solvus temperature and γ′ volume fraction were raised by individual additions of Ta and Ti, and increased further in the quinary alloy containing both alloying additions. In contrast to ternary and quaternary alloys, an improved microstructural stability with the stable γ–γ′ two-phase microstructure and more than 60% γ′ volume fraction existed in the quinary alloy after prolonged aging treatment at 1050°C for 1000 h. The creep behavior at 900°C revealed lower creep rates and longer rupture lives in the quaternary alloys compared to the ternary alloy, whereas the quinary alloy exhibited even better creep resistance. When the creep temperature was elevated to about 1000°C, the creep resistance of the quinary alloy exceeded the previously reported Co-Al-W-base alloys and first-generation Ni-base single-crystal superalloys. The improved creep resistance at approximately 1000°C was considered to be associated with high γ′ volume fraction, γ′ directional coarsening, and dislocation substructure, which included γ–γ′ interfacial dislocation networks and the sheared γ′ precipitates containing stacking faults and anti-phase boundaries.     

Phase equilibria and mechanical properties of the Ir–W–Al system

Phase equilibria in the Ir–W, Ir–Al and Ir–W–Al systems at temperatures between 1100 °C and 1600 °C were experimentally investigated using diffusion couples and two- or three-phase alloys, and the mechanical properties of γ′ (L1₂) strengthened Ir–W–Al alloys were examined by hardness and compression tests at room and elevated temperatures. The phase boundaries between the γ(A1)/ε′(D0₁₉), ε′/ε(A3) and ε/ε″(B19) in the Ir–W system at 1400 °C–1600 °C and those between the γ/β(B2) and β/Al_2.7Ir in the Ir–Al system at 1100 °C–1400 °C were determined. The phase diagrams in the Ir-rich corner of the Ir–W–Al ternary system at 1300 °C and 1400 °C were also determined. The existence of the γ′ phase of the Ir₃(W,Al) ternary compound was confirmed, and this system was found to consist of the γ, γ′, ε, ε′ and β phases in the Ir-rich portion. It was also found from hardness and compression tests up to 1200 °C that Ir–Al–W alloys having the γ + γ′ structure with a small lattice misfit show high hardness and strength at room and high temperatures.     

Phase chemistry of the superalloy SC16 after creep deformation

The local chemical concentrations of the elements in the nickel-based single crystal superalloy SC16 were examined by atom probe field ion microscopy (APFIM) after standard heat treatment and after creep strain of 1.35% at 1223 K. The measurements were carried out along the [001] direction parallel to the applied creep stress. An enrichment of Al and a slight depletion of Ti in the γ′ precipitate near the γ′/γ interface were observed in both states, the as-prepared and the creep-deformed. The average chemical composition of the γ′ precipitates had hardly been changed during the creep deformation. However, the average Cr content decreased in γ channels perpendicular to the applied stress significantly. Its enrichment was detected near the interface. Contrary to Cr, the average Ni concentration increased in these γ channels and depleted near the interface. Both Ti and Ta seem to be depleted in γ channels near the interface after creep deformation. According to the results, the long range diffusion for directional coarsening of γ′ precipitates is suggested to take place mainly in γ channels.     

Lattice strain evolution during creep in single-crystal superalloys

In situ neutron diffraction studies are carried out to characterize the micromechanical deformation occurring during tensile creep of a typical single-crystal nickel-based superalloy, CMSX-4. The loading responses of the matrix γ phase and the precipitate γ′ are distinct. Moreover, the behaviour in the tertiary creep regime (in which the γ′ phase remains intact) is qualitatively different from that in the primary creep regime (when γ′ is sheared). In tertiary creep, initial deformation of the matrix leads to a release of misfit between the phases in the (1 0 0), resulting in elastic compression of the γ in the loading direction. The load state then remains fairly constant during creep. During the initial stages of primary creep, elastic compression of the γ phase is observed until at around 2–4% creep strain this compression stabilizes as the (1 0 0) misfit is released. This is the point at which γ′ shearing is thought to begin. Subsequently, the load in the γ increases by around 200 MPa until a maximum is reached at around 8% creep strain. This load is then suddenly released, which may be due to the release of back-stress.     

Increase of misfit during creep of superalloys and its correlation with deformation

In superalloys the loss of coherency during creep results in the increase of misfit of the γ/γ′-interface. The kinetics of this process were measured locally by TEM (Moiré fringes) and X-ray diffraction. Two materials were creep tested (SRR99 and CMSX-4) in two temperature ranges (stable γ′-morphology and rafting), and the morphology changes were quantified. A microstructural model allows calculation of the equilibrium misfit and the increase of plastic strain on the basis of these data. At high temperatures and low stresses the model describes quantitatively creep kinetics up to 30 h. Here the processes controlling primary creep are propagation of dislocation loops along matrix channels and thickening of the matrix channels orientated perpendicular to the load direction.     

Re及温度对单晶镍基合金晶格常数及错配度的影响

通过对不同状态及不同Re含量单晶镍基合金进行高、低温X射线衍射谱线测定及组织形貌观察,研究Re含量及温度对单晶镍基合金中γ、γ′两相晶格常数及错配度的影响。结果表明:铸态合金中γ、γ′两相有较大的晶格常数及错配度;经完全热处理后,立方γ′相以共格方式嵌镶在γ基体中,合金中两相的晶格常数及错配度略有减小;长期时效使γ′相粗化后,两相之间出现界面位错,使合金中两相的晶格常数及错配度绝对值增加。随Re含量增加,合金中γ、γ′两相在室温的晶格常数增大,错配度的绝对值减小。与γ′相相比,γ基体相有较大的膨胀系数,因此,随温度提高,合金中两相晶格错配度的绝对值增大。     

Rafting mechanism for Ni-base superalloy under external stress: elastic or elastic–plastic phenomena?

Rafting mechanism in Ni-base single-crystal superalloys has been discussed with the total mechanical energy calculated for typical microstructures. We found that the actual rafting phenomena cannot be explained within the coherent elastic regime. The present calculations reveal that (i) only the transverse rafted structure with laminates normal to the stress direction can be realized, regardless of tensile or compressive stresses, and (ii) the lattice misfit is not relevant to the choice of the rafted structures. However, when the eigenstrain of the spherical (dilatational) symmetry changes into that of the tetragonal symmetry with misfit dislocations on the γ/γ′ interfaces, the signs of lattice misfit and external stress govern the choice of the transverse or longitudinal rafts. It is concluded that the rafting belongs to an elastic–plastic phenomenon.     

Mechanical properties and lattice misfit of γ/γ′ strengthened Co-base superalloys in the Co–W–Al–Ti quaternary system

A continuous γ/γ′ two-phase field has been identified extending between the ternary Co–Al–W system to the binary Co–Ti system. The lattice misfits of two phase γ/γ′ alloys from the Co–Al–W–Ti quaternary system were measured by X-ray diffraction and found to be positive and vary linearly with composition. Differential scanning calorimetry measurements showed that the solidus and liquidus temperatures decrease from the W and Al rich end to the Ti rich end, whilst the γ′ solvus temperature increases. Long term heat treatments identified the occurrence of discontinuous precipitation at the grain boundaries in many of the alloys studied. The high temperature strength and creep resistance of the quaternary alloys in the intermediate composition range surpassed those of the binary and ternary alloys.     

Neutron-diffraction study and modeling of the lattice parameters of a NiAl-precipitate-strengthened Fe-based alloy

The lattice misfit between the body-centered cubic α-Fe matrix and the B2-ordered NiAl-type β′ precipitates is a parameter of significant importance in controlling the creep resistance of precipitate-strengthened ferritic steels. However, the measurement of the lattice misfit is complicated due to the fact that the fundamental reflections of α and β′ phases almost completely overlap. In this study, neutron diffraction is used to determine the lattice parameters of these two phases in a Fe–18.9 Al–9.8 Cr–13 Ni–1.8 Mo (atomic percent, at.%) alloy as a function of temperature. The accuracy of the measurement at room temperature is verified by high-energy synchrotron X-ray diffraction. The comparison between these two techniques is discussed in terms of the difference in superlattice intensity. Furthermore, using the phase compositions determined by atom probe tomography, models are proposed to predict the lattice parameters of both phases at room temperature as a function of their compositions. The results are in very good agreement with those obtained experimentally.     

Hf含量对FGH97合金γ/γ′晶格错配度的影响

采用X射线衍射(XRD)方法测算镍基粉末冶金高温合金FGH97中γ和γ′相的晶格常数,计算出γ/γ′晶格错配度。结果表明:γ′相的晶格常数比γ相的小,错配度为负值。Hf 主要存在于γ′相中,随着合金中 Hf 加入量的增加,进入γ′相中 Hf 的数量增加,使γ′相的晶格常数逐渐增大,错配度的绝对值逐渐减小。     

Role of Ru on the Microstructural Evolution During Long-Term Aging of Ni-Based Single Crystal Superalloys

Two experimental alloys containing different contents of Ru were investigated to study the effect of Ru on the microstructural evolution during long-term thermal exposure. The increase in Ru promoted the formation of cubical, tiny, and even γ′ phase after full heat treatment. Moreover, the samples after full heat treatment were exposed at 1100 °C for different time. Based on the classical model by Lifshitz, Slyozov, and Wagner, the coarsening of γ′ phase of the alloy containing 2.5 and 3.5 wt.% Ru during the long-term aging was controlled by the interface reaction and diffusion, respectively. The γ/γ′ lattice misfit was more negative with the increment of Ru addition, which induced the formation of stable rafted γ′ phase in the alloy containing 3.5 wt.% Ru at the initiation of long-term aging. Besides, the increase in Ru reduced the diffusion coefficient, which could restrain the γ′ phase coarsening. The lower γ/γ′ lattice misfit of the alloy containing 2.5 wt.% Ru promoted the interface reaction, which induced the rapid coarsening of γ′ phase. Therefore, the increase in Ru improved the microstructural stability of the alloys. On the other hand, the raise of Ru induced “reverse partitioning” behavior, which was effective in suppressing the emergence of the topologically close-packed phase (TCP phase). The TCP phase occasionally occurred in the alloy containing 2.5 wt.% Ru, which was attributed to the high temperature and the supersaturation of the γ matrix. Moreover, the TCP phase was determined as μ phase, which had a high concentration of Co, Re, Mo, and W. A sketch map describing the evolution of the TCP phase was also constructed.     

Phase-field modeling of the γ′-coarsening behavior in Ni-based superalloys

Microstructural changes during heat treatment of the Ni-based CMSX-4 and CMSX-6 superalloys have been investigated experimentally and simulated using a phase-field multi-component model incorporating elastic driving forces in the presence of a lattice misfit. Furthermore, a theoretical model of the coarsening of anisotropic particles is proposed for the prediction of the main kinetic parameters of the coarsening process. A comparison of the main characteristics of the microstructural evolution during non-directional γ′-coarsening, provided from both experiments and phase-field simulations, gives a good agreement of the coarsening kinetics of the CMSX-4 superalloy. However, for the CMSX-6 superalloy, phase-field simulation results and theoretical predictions are not entirely consistent with experimental results, and show that additional effects, for example, those caused by plastic deformation, might be a reason for the slow coarsening rate.     

Microstructural characterization in 7 at% Al-containing NiTi-based alloys

The microstructural evolution of Ni–42Ti–7Al and Ni–41Ti–7Al alloys as a function of solution and aging heat treatment was investigated using transmission electron microscopy（TEM）, electron probe, and X-ray diffraction（XRD）. The results reveal that the volume fraction of Ti2 Ni phase as well as its composition does not change significantly after as-solution treated at 1200 °C and aged at 850 °C. At the early stage of the aging treatment at 850 °C for 1 h, the cuboidal β＇ precipitate keeps coherency with the matrix; further aging, β＇ precipitate coarsens, and the semicoherency between the β/β＇ two phases are observed.The shape of coarsened β＇ precipitates changes to the globule, and the interface dislocations are introduced accompanied by the occurrence of semicoherent precipitates. Under the same heat treatment, compared to the Ni–42Ti–7Al alloy, the lattice misfits of the Ni–41Ti–7Al alloy between the β and β＇ two phases are larger, so the β＇ precipitates in Ni–41Ti–7Al alloy are coarsened severely and easily lose coherency with the matrix. The thermal stability of Ni–41Ti–7Al alloy is much worse when aging at 850 °C.     

热处理工艺对一种新型铸造镍基高温合金的组织和性能影响

通过改变固溶热处理温度、保温时间和固溶后冷却方式,研究了不同固溶热处理工艺对一种新型铸造高温合金组织和性能的影响.结果表明,将合金在不同温度固溶处理2 h后空冷,合金在760℃,660 MPa和980℃,180 MPa条件下的持久寿命随热处理温度的升高先升高而后降低;固溶处理温度为1220℃时,760℃,660 MPa条件下的持久寿命达到最高;固溶处理温度为1180℃时,980℃,180 MPa条件下的持久寿命最高;当热处理温度从1120℃升高到1220℃时,拉伸强度随温度升高而增加,继续升温到1240℃,拉伸强度下降.当固溶热处理温度为1120℃,处理时间在2-8 h范围内变化时,合金在760℃,660 MPa条件下的持久寿命随时间延长而降低,而在980℃,180 MPa条件下的持久寿命随处理时间延长而升高;当热处理时间为2和4 h时,拉伸强度较高;延长到6和8 h时,拉伸强度下降.当冷却方式不同时,合金持久性能也发生变化.γ′相和γ/γ′共晶组织在尺寸、形态、分布和数量上的变化是导致合金力学性能变化的关键因素.     

Evolution of interfacial dislocation networks during long term thermal aging in Ni-based single crystal superalloy DD5

Interfacial dislocations found in single crystal superalloys after long term thermal aging have an important effect on mechanical properties. Long term thermal aging tests for DD5 single crystal superalloy were carried out at 1,100 ℃ for 20, 100, 200, 500 and 1000 h, and then cooled by air. The effect of long term thermal aging on the dislocation networks at the γ/γ' interfaces was investigated by FE-SEM. Results showed that during the long term thermal aging at 1,100 ℃, misfit dislocations formed firstly and then reorientation in the(001) interfacial planes occurred. Different types of square or rectangular dislocation network form by dislocation reaction. Square dislocation networks consisting of four groups of dislocations can transform into octagonal dislocation networks, and then form another square dislocation network by dislocation reaction. Rectangular dislocation networks can also transform into hexagonal dislocation networks. The interfacial dislocation networks promote the γ' phase rafting process. The dislocation networks spacings become smaller and smaller, leading to the effective lattice misfit increasing from-0.10% to-0.32%.