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- HIP (4)
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- Electron backscatter diffraction (2)
- Electron microscopy (2)
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- Ni-base superalloy (2)
Organisationseinheit der BAM
Методом рентгеноструктурного анализа в интервале температур 18—1150 °С определены температурные зависимости периодов кристаллических решеток γ- и γ'-фаз, их размерно-го несоответствия (мисфит) и объемной доли γ'-фазы экспериментального монокристал-лического жаропрочного никелевого сплава. Определены диапазоны температур, в которых происходят интенсивные изменения структурно-фазовых характеристик исследованного сплава.
Electron microscopy investigation of the structure of a compact extruded from nanopowder of nickel
(2007)
Initially, as-cast and homogenized single crystals of nickel-base superalloy CMSX-4 are subjected to hot isostatic pressing at 1288 °C. Two series of experiments are conducted: 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 is investigated metallographically and by high-resolution synchrotron X-ray tomography. The obtained experimental results are compared with the predictions of the vacancy model proposed recently in the group. Herein, the model is 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 are used for selecting the optimal technological parameters such as applied pressure and processing time
Synthesis of Molybdenum and Niobium Mono- and Binary Silicides by the Method of SHS-Metallurgy
(2016)
The process of self-propagating high-temperature synthesis of the Mo–Nb–Si silicides from the powder mixtures has been investigated. Based on performed experiments, the composition of powder mixtures as well as technological parameters are proposed which provide the synthesis of monosilicides MoSi₂, NbSi₂, and binary silicides Mo₁-хNbxSi₂ with different ratios of Nb/Mo by adding different contents of MoO₃ and Nb₂O₅. Microstructure and phase compositions of the obtained silicide ingots are characterized by scanning electron microscopy, electron probe microanalysis, X-ray diffraction, and backscatter electron diffraction.
Mechanism of porosity growth during homogenisation in single crystal nickel-based superalloys
(2013)
Several mechanisms for porosity growth in single crystal nickel-based superalloys during homogenisation heat treatment have been proposed in the literature. They were carefully checked using different experimental methods, namely quantitative light microscopy, scanning electron microscopy, transmission electron microscopy, X-ray diffraction and density measurements. It is shown that the main mechanism is the Kirkendall–Frenkel effect, i.e. generation of voids due to uncompensated efflux of Al atoms from dissolving γ/γ′-eutectic areas. The Al diffusion is supported by the afflux of vacancies from surrounding γ-matrix which results in porosity growth. This conclusion is confirmed by the estimation of the vacancy afflux towards the dissolving eutectic.
The thermal stability of the microstructure of a heat-resistant cobalt alloy, which consists of a γ solid solution strengthened with γ'-phase precipitates, has been studied. The temperature behavior of the dissolution of the hardening γ' phase and the kinetics of its coarsening at 700 and 800°C have been determined. It is found that, during prolonged annealing at 800°C, the γ' → β phase transformation occurs.
The competitive growth of columnar grains in a single-grain selector, which is used for directional solidification of single-crystal blades from nickel-based superalloys, has been investigated by electron backscattered diffraction and local X-ray diffraction analysis. It has been found that the competitive grain growth in a starter block is determined by the crystallographic factor: rapidly growing grains with the axial orientation close to the [001] direction dominate in this part of the casting. For the competitive grain growth in a helicoidal separator, the geometric factor (the position of a grain at the input of the separator) is also important. The results obtained suggest that an appropriate geometry of the single-grain selector was chosen. In addition, the distribution of the orientations of columnar grains obtained by electron backscattered diffraction, can be used for approximate estimation of the yield of suitable (i.e., with the deviation of the axial orientation from the [001] direction within a specified tolerance) single-crystal blades.
Mit Hilfe des HIP-Verfahrens („Hot Isostatic Pressing“) werden Poren in der einkristallinen Nickel-Basis Superlegierung CMSX-4 kontinuierlich geschrumpft und dadurch die nach der Erstarrung und der Wärmebehandlung vorhandene Porosität stark reduziert. In diesem Beitrag werden experimentelle und numerische Untersuchungen zu den Mechanismen der Porenschrumpfung zusammengefasst. Es zeigt sich, dass das Verformungsverhalten während Kriechversuchen bei der HIP-Temperatur durch Versetzungsgleitung auf oktaedrischen Ebenen dominiert wird.
Dagegen zeigen Messungen der Porositätsabnahme und Simulationen des Porenschließens, dass die Kinetik der Porenschrumpfung durch das Phänomen der Leerstellendiffusion zwischen Poren und Kleinwinkelkorngrenzen („Low Angle Boundary“, LAB) bestimmt wird. Im Gegensatz führt die klassische Kristallviskoplastizität zu einer systematischen Überschätzung dieser Kinetik. Der scheinbare Widerspruch lässt sich auflösen, wenn man bedenkt, dass auf der Skala der Poren Versetzungsquellen nicht gleichmäßig verteilt sind, wie in der konventionellen Kristallplastizität implizit angenommen wird. Stattdessen wird in einem weiterführenden Modell davon ausgegangen, das Kleinwinkelkorngrenzen (LABs) als Versetzungsquellen fungieren, während die Scherspannungen sehr stark in der Nähe der Poren lokalisiert sind, was die Emission von Versetzungen deutlich reduziert.
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 gamma and gamma' phases were predicted.
This prediction was supported by measurement of the temperature dependence of the gamma'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.
Pore annihilation was investigated in the single-crystal nickel-base superalloy CMSX-4. HIP tests at 1288 °C/103 MPa were interrupted at different times, then the specimens were investigated by TEM, metallography and density measurements. The kinetics of pore annihilation was determined. The pore closure mechanism was identified as plastic deformation on the octahedral slip systems. A model describing the kinetics of pore closure has been developed on the base of crystal plasticity and large strain theory. Mechanical tests with the superalloy CMSX-4 and the Ru-containing superalloy VGM4 showed, that HIP significantly increases the fatigue life at low temperatures but has no effect on creep strength.
The morphology of pores partially shrunk during a half-hour HIP at temperature of 1288 °C and pressure of 103 MPa has been investigated in nickel-based superalloy CMSX-4. The investigation resulted in the following findings: surrounding the shrinking pores by a c¢-shell (Ni3Al), faceting of the pores surface by {023} and {011} planes, and formation the submicroscopic satellite pores connected by channels with the neighboring larger pores. It is assumed that the formation of the c¢-shell around the pores and the faceting of the pore surface is due to diffusion processes occurring during pore shrinkage, and therefore these findings can be considered as arguments supporting the vacancy model of pore annihilation. The submicroscopic satellite pores are expected to be the result of dividing the casting pores of a complex initial shape during their shrinking. The connecting channels are probably required for the gas to escape from the rapidly shrinking small satellite pores into the slowly shrinking large pore. Thus, it is reasonable to assume that the casting pores may contain some amount of gas.
Pore annihilation during hot isostatic pressing (HIP) was investigated in the single-crystal nickel-base superalloy CMSX-4 experimentally by interrupted HIP tests at 1288 °C/103 MPa. The kinetics of pore annihilation was determined by density measurement and quantitative metallography. Transmission electron microscopy of a HIPed specimen showed that the pores shrink via dislocation movement on octahedral glide planes. Theoretically pore closure under HIP condition was modelled by the finite element method using crystal plasticity and large strain theories. The modelling gives a similar kinetics of pore annihilation as observed experimentally, however somewhat higher annihilation rate.
Data about the creep behaviour of metals and their alloys at temperatures close to the melting point are very limited. The reason is that most engineering alloys are used at temperatures below 0.6-0.8 of their melting point, so, Investigation of creep at higher temperatures has no practical relevance. For some special applications however it is important, in our case hot isostatic pressing (HIP) of single-crystal turbine blades cast from nickel-base superalloys. In order to remove porosity the blades are HlPed at temperatures between y'-solvus and solidus where superalloy has no strengthening y'-phase and therefore is very soft. For example, the Company Howmet Castings HIPs the superalloy CMSX-4 at the temperature 1288aC, which corresponds to a homologous temperature of about 0.97=1561 K/1612 K (solidus temperature). Therefore knowledge about the creep behaviour of CMSX-4 at this temperature and understanding of the creep mechanisms are necessary to model the kinetics of pore closure during HIP as well as to plan the Parameters of the HIP process.