Abstract
The effect of different solution treatments on the microstructure and element segregation of AM3 nickel-based single crystal superalloys with the carbon content of 0.045wt% was investigated. The optical microscope (OM) and scanning electron microscope (SEM) were used to observe the microstructure and γ' phase of AM3 superalloys, and the electron-probe microanalysis (EPMA) was used to analyze the element segregation. The results show that the incipient melting temperature of the AM3 superalloys is 1305 °C. After the solution treatment of 1305 °C/6 h following the homogenization treatment of 1300 °C/3 h, the incipient melting structure is reduced, and the incipient melting temperature is increased by about 5 °C. With increasing the solution temperature and prolonging the solution duration, the volume fraction and size of the precipitated γ' phase are increased significantly, and the segregation ratio of Cr, Co, Mo, W, and Al elements is closer to 1. The existence of incipient melting structure prevents the segregation of Ti in AM3 superalloys with prolonging the solution duration after heat treatment. Thus, the optimum heat treatment process is 1300 °C/3 h+1305 °C/6 h/air cooling (AC)+1080 °C/6 h+870 °C/20 h/AC. The dendrite structure of AM3 single crystal superalloys completely disappear after heat treatment. The cubic degree of γ' phase is improved, the size of γ' phase reaches 454 nm, the volume fraction of γ' phase is 66.05vol%, and the segregation of Cr, Co, Mo, W, Al, and Ti elements is significantly reduced.
Science Press
Nickel-based single crystal superalloys have wide applications in gas-turbine engine due to their high-temperature bearing capacity and superior mechanical propertie
The effects of heat treatment process on the microstructure of Ni-based superalloys have been investigate
Kubin et a
Therefore, the effect of different heat treatments on the microstructure and element segregation was studied in this research, and it provided a theoretical basis for the development and application of the single crystal superalloys.
The chemical composition of the nickel-based AM3 superalloys is shown in
The heat treatments were performed in SX2-9-17TP type high temperature furnace with the temperature fluctuation of ±1 °C. The γ' phase has the solvus temperature, liquidus tem-perature, and solidus temperature of 1293.5, 1329.2, and 1361.0 °C, respectivel
In order to observe the dendrite structure and γ' phase of the alloys, the as-cast alloy and the specimens after heat treatment were ground, polished, and etched by 10 mL HNO3+20 mL HF+30 mL C3H8O3.
The dendrite structure of AM3 superalloys was observed by an OLYMPUS-GX71 optical microscope (OM). The dendrite arm spacings were measured by Image J software. The γ' phase was observed by a S-4800 scanning electron microscope (SEM). The mean size and the volume fraction of γ' phase were measured by Image J software.
Element segregation was analyzed by JXA8100 electron probe microanalysis (EPMA). It was difficult to specify the dendrite core (DC) and the interdendritic area (IA) due to the elimination of dendrite structure after heat treatment. Thus, In order to study the element segregation of AM3 superalloys after heat treatment, the point scanning matrix techniqu

Fig.1 Microscope image for element segregation determination by point scanning matrix technique
The residual segregation ratio k was defined as follows:
(1) |
where m is the total number of points in DC area; n is the total number of measured points; and are the components of each point in DC and IA, respectively. The content at each point and the average content were used to divide the dataset into DC and IA parts, respectively. The points with greater contents of positive segregation elements (Al, Ti, and Ta) than the average content were considered as IA part, whereas those with smaller contents of positive segregation elements were considered as DC part. The points with greater contents of negative segregation elements (Co and W) than the average content were considered as DC part, while the points with smaller contents of negative segregation elements than the average content were considered as IA par

Fig.2 Transverse (a) and longitudinal (b, c) interface morphologies of as-cast AM3 superalloys

Fig.3 OM microstructures of AM3 superalloy specimens after different heat treatments: (a) HT1, (b) HT2, (c) HT3, (d) HT4, (e) HT5, (f) HT6, and (g) HT7
It is well known that the γ matrix has fcc structure and the γ' phase has fcc-like structure. Their lattice mismatch is very small and the solute supersaturation is high, which is conducive to the nucleation of the γ' phase from γ supersaturated solid solutio

Fig.4 Microstructures of γ' phase after casting (a) and different heat treatments (b~h): (b) HT1, (c) HT2, (d) HT3, (e) HT4, (f) HT5, (g) HT6, and (h) HT7

Fig.5 Size of γ' phase in AM3 superalloys after casting and different heat treatments

Fig.6 Volume fraction of γ' phase in AM3 superalloys after casting and different heat treatments
The high temperature rupture property of nickel-based single crystal AM3 superalloys is related to the shape, volume fraction, and size of the γ' phase. The good cubic degree and large volume fraction of γ' phase both contribute to the improvement in alloy properties. The effect of γ' phase size on the properties is particularly important due to the interaction between the γ' phase and dislocations. Under the high temperature and low stress, the dislocations bypass the γ' phase. When the γ' phase size is large, the path of the dislocations to bypass the γ' phase will be extended. Besides, the regular γ' phase is conducive to the rapid formation of raft structure. These are all enhancement mechanisms for the high temperature rupture property of alloys. However, when the heat treatment temperature is too high, the raft thickness of γ' phase is overly increased, which is disadvantageous for the high temperature rupture property of alloys. Therefore, it is extremely important to form a γ' phase with an appropriate size. Ref.[
The degree of element segregation under different heat treatments is shown in

Fig.7 Negative segregation ratio k of AM3 superalloys after different heat treatments

Fig.8 Positive segregation ratio k of AM3 superalloys after different heat treatments
The solution temperature is the most important factor for the element diffusion rate. The higher the solution temperature, the larger the thermal activation energy of the atoms and the faster the atom migration.
(2) |
where D is the diffusion coefficient, D0 is the diffusion constant, Q is the diffusion activation energy per mole atom, R is a gas constant of 8.314 J·mo
In addition, the solution duration is also an important influence factor. The degree of element segregation is analyzed by the homogenization kinetic equation or the residual segregation coefficient (δ
(3) |
where and are the highest and lowest concentrations of elements after the solution for t h, respectively; and are the highest and lowest concentrations in the initial state, respectively. Ref.[
(4) |
where C(x) represents the element concentration at the position of x (x=0~λ); C is the average concentration; λ is the dendrite arm spacing; ΔC0 is the difference between the highest/lowest concentration and the average concentration; t is the solution duration. Therefore, the residual segregation coefficient δ can be obtained by
(5) |
It can be seen that the diffusion coefficient and the distance in IAs are constant. Thus, the longer the solution duration, the smaller the residual segregation δ and the better the solution effect of the alloys.
1) The dendrite structures of single crystal AM3 superalloys with 0.045wt% carbon are significantly reduced or even disappear after heat treatment, and the eutectic structures are significantly reduced. The AM3 superalloys undergo three processes with increasing the solution temperature: the dendritic structures are not completely eliminated→the dendritic structures are completely eliminated without incipient melting→the incipient melting occurs. The incipient melting temperature of the alloy is 1305 °C. The homogeni-zation treatment of 1300 °C/3 h before the heat treatment of 1305 °C/6 h reduces the volume fraction of the incipient mel-ting structure, and the incipient melting temperature is increased by 5 °C.
2) The γ' phase shows an irregular butterfly shape with uneven arrangement and distribution in the as-cast AM3 superalloys, whereas that shows the cubic and stripe shape with more uniform arrangement and distribution in AM3 superalloys after heat treatment. The size and volume fraction of γ' phase in alloys after heat treatment are significantly increased. With increasing the solution temperature and prolonging the solution duration, the coarse γ' phase is fully dissolved in the matrix, and the volume fraction and size of the precipitated γ' phase are increased significantly during the subsequent cooling process.
3) The segregation ratio of Cr, Co, Mo, and W is greater than 1, and that of Al and Ti is less than 1 of AM3 superalloys after heat treatment. With increasing the solution temperature and prolonging the solution duration, the segregation ratio of Cr, Co, Mo, W, and Al is closer to 1, and the element diffusion becomes more sufficient. The existence of incipient melting structure prevents the segregation ratio of Ti in the alloy from changing regularly with prolonging the solution duration.
4) The optimum heat treatment for AM3 superalloy is 1300 °C/3 h+1305 °C/6 h/air cooling (AC)+1080 °C/6 h+ 870 °C/20 h/AC. The dendrite structures are completely elimi-nated, and no incipient melting occurs. The γ' phase of 454 nm in size and 66.05vol% in volume fraction has a better cubic degree with a uniform arrangement and distribution. The degree of segregation of Al, Ti, Cr, Co, Mo, and W is significantly reduced.
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