Gamma Prime Phase Stability after Long-Term Thermal Exposure in Cast Nickel Based Superalloy, IN-738

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1 312 Chiang Mai J. Sci. 2009; 36(3) Chiang Mai J. Sci. 2009; 36(3) : Contributed Paper Gamma Prime Phase Stability after Long-Term Thermal Exposure in Cast Nickel Based Superalloy, IN-738 Panyawat Wangyao* [a], Nutthida Chuankrerkkul** [b], Sureerat Polsilapa [c], Ponlit Sopon [c] and Weerasak Homkrajai [d] [a] Department of Metallurgical Engineering, Faculty of Engineering, Chulalongkorn University, Bangkok 10330, Thailand. [b] Metallurgy and Materials Science Research Institute, Chulalongkorn University, Bangkok 10330, Thailand. [c] Department of Materials Engineering, Faculty of Engineering, Kasetsart University, Bangkok 10900, Thailand. [d] Electricity Generating Authority of Thailand, Nonthaburi 11130, Thailand. *Author for correspondence; panyawat@hotmail.com; nutthita.c@chula.ac.th Received: 13 January 2009 Accepted: 20 March 2009 ABSTRACT Long-term isothermal exposure tests were conducted on IN-738 alloy to evaluate the variation of gamma prime particle coarsening behavior after different rejuvenated heat treatment conditions. The long-term exposure tests (up to 2,500 hours) were conducted at two temperatures (900 o C and 1,000 o C) to assess gamma prime particle coarsening behavior. Metallographic work was performed on isothermally aged samples to characterize gamma prime coarsening as a function of aging time and temperature. At all aging temperatures and/ or times investigated, the gamma prime particles in all tested specimens were more coarsening than the initial reheat treated ones. The gamma prime particles appeared to be more coarsening into round shape or agglomerated between them comparing to the initial ones of each reheat treatment. The degree of coarsening, as evidenced by gamma prime particle size, increased with increasing heating time and temperature. In most cases, the amount of secondary or very fine gamma prime precipitates decreased with increasing heating temperature and finally disappeared. It was found that the lower solutioning temperature provided the higher rate of γ coarsening at both elevated temperatures. In contrast, the higher solutioning temperature kept slow rate of γ coarsening resulting in lower average γ particle size. Keywords: rejuvenation, re-heat treatment, microstructural repair, gamma prime particle coarsening, and nickel-based superalloy. 1. INTRODUCTION Nickel based superalloys are structural materials with chemical composition and structure, which have been developed to enable the use at high temperature applications. The microstructures and mechanical properties (for both low and high temperatures) can be related to their manufacturing processes. One of these processes is heat treatment, which solution treatment in most cases, followed by a single or a double aging sequence to

2 Chiang Mai J. Sci. 2009; 36(3) 313 precipitate homogeneous distributions of either cuboidal or spherical gamma prime within the grains interior as well as discrete grain boundary carbides [1]. Full solution treatment or partial solution treatment temperatures including aging treatments have been developed and modified to optimize the completed precipitation of gamma prime phase in matrix. The size, volume fraction and distribution of gamma prime phase are vital to control the creep strength at high to intermediate stresses. The proper reheat-treated microstructure can provide their phase stability, and adequately high strength and good ductility even after long-term thermal exposure. The mechanical property behaviors of superalloys are very strongly related to the alloy microstructures [2-6]. The superalloy microstructures continually change with time at the elevated temperatures. In the new, heat treated alloy, the gamma prime (γ ) particles are arranged in a structure, which results in an optimum balance of tensile, fatigue, and creep properties [7-10]. It is generally known that mechanical properties are related to the microstructures. Therefore, many previous research works [3-11] had been carried out to investigate the relationships of microstructure and mechanical properties. However, the use of these expensive materials requires a repair process providing the re-establishment of the initial properties and the original microstructure of the longterm used or damaged parts for the economic reason. The heat-treatment processes for nickel-based superalloys continue to change in order to optimize numerous mechanical and physical properties [5-9]. This allows making the selection of heat treatment parameters increasingly challenging. The cast nickel-based superalloy IN-738 is used as a blade material in the first row high-pressure stage of gas turbines. The alloy contains refractory elements such as Mo, W, Ta, Cr and Co to prevent local hot corrosion [10]. The alloy has a multi-phase microstructure consisting FCC γ matrix, bimodal γ precipitates (primary and secondary), γ-γ eutectic, carbides and a small amount of deleterious phases such as σ, δ, η and Laves. The total weight percent of γ in IN-738 superalloy is higher than 60% [11]. Therefore, the high-temperature strength of the alloy depends strongly on γ properties. According to the previous work [12], the rejuvenation process provides blades to double and, in some cases, triple the lifetime as compared to the original ones. For alloys such as IN-738, IN-792, U-500, X-750 and the newer alloys such as GTD 111, GTD- 111DS, R80DS, and IN-939, which are used in many land-based gas turbines, have been rejuvenated and successfully returned to service according to the previous information of LIBURDI Engineering Company Limited, Canada. In each case, the blades were creep life expiry when received for processing and then giving reliable service after rejuvenation. The aim of this research work is to determine the most suitable and practicable repair-condition, which could restore microstructure and provide the most microstructural stability after long-term thermal exposure for gas turbine blades made of casting nickel based superalloy grade IN-738 after 50,000-hour service operated by Electricity Generating Authority of Thailand (EGAT). 2. MATERIALS AND METHODS The cast nickel base superalloy in this study was IN-738 (see chemical composition in Table 1). Rectangular plates, having a dimension about 1 cm 2 were cut from the most severe degradation zone of turbine blades. Specimens were heat treated according to heat treatment conditions including solution treatment, primary and secondary precipitation aging treatments in vacuum furnace. The details of

3 314 Chiang Mai J. Sci. 2009; 36(3) experimental heat treatments are shown in Table 2. Then reheat treated specimens after each condition were heated at both 900 o C and 1,000 o C for 500, 1000, 1500, 2000, and 2500 hours in order to investigate the coarsening behavior of gamma prime particles after various reheat treatments. All sectioned samples after each aging Table 1. Chemical composition in weight % of IN-738. Ni Cr Co Ti Al W Mo Ta Nb C Fe B Zr Bal Table 2. Heat treatment conditions applied to long term exposed IN-738. Condition Solution Primary Secondary No. Treatment precipitate aging precipitate aging 1 * 1125 o C/ 2hr. (AC) o C/ 24 hr. (AC) o C/ 2hr. (AC) 925 o C/ 1 hr. (AC) 845 o C/ 24 hr. (AC) o C/ 2hr. (AC) 1055 o C/ 1 hr. (AC) 845 o C/ 24 hr. (AC) o C/ 2hr. (AC) o C/ 24 hr. (AC) o C/ 2hr. (AC) 925 o C/ 1 hr. (AC) 845 o C/ 24 hr. (AC) o C/ 2hr. (AC) 1055 o C/ 1 hr. (AC) 845 o C/ 24 hr. (AC) * Standard Heat-Treatment condition. were ground and polished using standard metallographic techniques and were subsequently etched in marble etchant. The etchant s chemical compositions are: 10 g. CuSO 4, 50 ml HCl, and 50 ml H 2 O. The microstructures of heat treatment samples were study by scanning electron microscope with secondary electron mode and Image Analyzer. The size and volume fraction of gamma prime particles were determined. 3. RESULTS AND DISCUSSION 3.1 As-received Microstructure The SEM photograph, obtained from the transverse sections at about mid blade height of the airfoil, is shown in Figure 1a. The microstructure of as-cast alloy generally consists of extensive precipitation of ordered L1 2 γ intermetallic phase within dendrite core and in the interdendritic region. The agglomerated gamma prime particles can be seen. Coalescence of the primary and secondary gamma prime particles, as result of long-term service, seems to occur resulting in larger and rounded particles. However, carbide and/or gamma prime phases normally lowers ductility or toughness of blade alloy. This can lead to lower creep strength and impact resistant of the blades. In this study, the airfoil microstructure showing significant degradation in service, the coarse gamma prime particle size was about 1.2 micron. The primary gamma prime particles have spheroidized and secondary gamma prime coarsened in the airfoil samples. This type of microstructure is theoretically expected to have low efficiency to block dislocation movements during loading at high temperatures resulting in lower creep resistance. Therefore, it is needed to recover

4 Chiang Mai J. Sci. 2009; 36(3) 315 microstructure to the same as or similar to the original one by simple reheat treatment processes. 3.2 The Microstructures of Reheat-treated Alloy According to the previous works [7-8, 13], repeating the standard heat treatment sequence does not always work well. The structure and properties were not fully recovered by this refurbishment treatment applied to these IN-738 blades. It is reported that the microstructure was only partially recovered by such simple reheat treatment. However, when reheat treatment condition, according to No.1 (standard heat treatment), was applied to long-term exposed specimen in this study, the more homogeneous microstructure consisting of uniform dispersion of finer gamma prime precipitates was obtained. The size of γ precipitate particles are uniform and similar in size and shape, Figure 1b. This type of microstructure is previously expected and theoretically desired as the most optimized microstructure, which could provide very good mechanical properties at elevated temperatures, especially, for both short-term strength at elevated temperature and high creep resistance. According to heat treatment of program No.2, It was found that the morphology is different from the standard heat-treated one. Primary precipitate aging at 925 o C for 1 hour resulted in an early precipitation of gamma prime γ particles. After secondary precipitate aging, elements needed to form γ precipitate would more diffuse into the former gamma prime precipitates causing the coarsening of these precipitates during secondary aging resulted in coarser size. Such kind of microstructure could probably provide good rupture and/or creep resistance in some degree. As it is already well known that creep strength of alloys by γ precipitation is a function of γ particle size. It can be concluded that temperature of 925 o C as primary aging produced more uniform and coarser of rounded-γ particles. The microstructure after heat treatment according to program No.3 shows the bimodal microstructure of non-uniform dispersion of both coarse and very fine gamma prime precipitates. The coarse gamma precipitates are in round shape at the proper size. Effect of primary precipitate aging at 1,055 o C for 1 hour resulted in more coarsening of both sizes of gamma prime particles with higher volume fraction of γ -phase after secondary aging comparing to the reheat-treated microstructure of programs No. 1 and 2, which has lower amount of precipitated coarsening particles. Specimens from programs No. 4-6 received the effect of the highest solutioning temperature on final microstructures. This highest solutioning temperature provided the microstructure with much lower driving force for coarse γ phase precipitation during aging resulting in very low volume fraction of coarse γ precipitated particles. The inserted primary aging could not strongly influence to the size, distribution and volume fraction of coarse γ particles but do greatly to the very fine one. 3.3 Microstructures after Long-term Exposures Heating at both temperatures resulted in drastically coarser gamma prime particles as compared to the initially received reheat-treated specimens as shown in Figures 1c and 1d, and presented by conditions 1-6 in Figures 2-5, which are referring to condition No. 1-6 in Table 2, respectively. However, in Figures 1c, 1d, 2 and 4, it could be clearly seen that the higher heating temperature of 1,000 o C provided the much higher coarsening rate of gamma prime particles than of the lower one (900 o C) due to the difference in kinetics. The

5 316 Chiang Mai J. Sci. 2009; 36(3) gamma prime particles greatly more coarsened into round shape than those in each initially reheat treated specimens. In the alloy, the degree of coarsening, as determined by gamma prime particle size, increased with both increasing heating temperature and time. At each heating temperature, the size of gamma prime particles increased, and the area fraction of gamma prime particle decreased with increasing heating time. It was also observed that an increasing heating temperature resulted in lower amount of gamma prime precipitation. During long-term heating, secondary gamma prime particles would dissolve into the matrix and then diffused to agglomerate with the coarse gamma prime particles. Considering the coarsening behavior of gamma prime particles at 900oC and 1,000oC (Figures 2 and 4), it was found that the microstructures under previous reheat treatment of conditions No. 5 was the most stable ones due to the slowest coarsening rate of gamma prime particles. When considering Figures 3 and 5, it could be seen that the area fraction of total gamma prime particles of specimen (a) (b) (c) (d) Figure 1. SEM micrographs of a) As-received microstructure after long-term service, b) After standard heat-treatment at 1,125oC / 2hr. (AC) and 845oC / 24 hr. (AC); Condition No. 1, c) After long-term exposure at 900oC for 2,500 hours; Condition No. 1 and d) After long-term exposure at 1,000oC for 2,500 hours; Condition No. 1.

6 Chiang Mai J. Sci. 2009; 36(3) 317 under all reheat treatment conditions continuously decreased with heating time. It was also found that the higher heating temperature of 1,000 o C resulted in faster reduction of area fractions of gamma prime particles comparing to those of the lower temperature ,000 1,500 2,000 2,500 3,000 Heating time (hr) Figure 2. The relationship between heating time and average size of gamma prime particles at 900 o C ,000 1,500 2,000 2,500 3,000 Heating time (hr) Figure 3. The relationship between heating time and average area fraction of precipitated phase at 900 o C.

7 318 Chiang Mai J. Sci. 2009; 36(3) ,000 1,500 2,000 2,500 3,000 Heating time (hr) Figure 4. The relationship between heating time and average size of gamma prime particles at 1,000 o C ,000 1,500 2,000 2,500 3,000 Heating time (hr) Figure 5. The relationship between heating time and average area fraction of precipitated phase at 1,000 o C. 4. CONCLUSIONS 1. The reheat-treated microstructure according to program No. 5 provided the most precipitated phase stability in term of minimum coarsening rate after long-term exposure at both 900 o C and 1,000 o C. 2. In almost reheat-treated microstructures, average area fractions of gamma prime phase clearly decreased with heating time.

8 Chiang Mai J. Sci. 2009; 36(3) 319 REFERENCES [1] Jackman L.A., Forming, Fabrication and Heat Treatment of Superalloys, in Superalloys Source Book, ASM, 1984: [2] Zrnik J., Wangyao P., Vrchovinsky V., Hornak P. and Mamuzic I., Deformation behaviour of wrought nickel base superalloy in conditions of thermomechanical fatigue, Metallurgija, 1997; 36: [3] Zrnik J., Semenak J., Vrchovinsky V. and Wangyao P., Influence of hold period on creep-fatigue deformation behaviour of nickel base superalloy, Mater. Sci. Eng., A, 2001; 319: [4] Kvackaj T., Zrnik J., Vrchovinsky V. and Wangyao P., Controlled rolling of Hastelloy-N, High Temp. Mater. Processes, 2002; 21: [5] Lothongkum G., Khuanleang V., Hromkrajai W. and Wangyao P., Effect of aging on stress relaxation of Inconel X-750 bolt at 923 and 1033 K, High Temp. Mater. Processes, 2006; 25: [6] Wangyao P., Krongtong V., Panich N., Chuankrerkkul N. and Lothongkum G., Effect of 12 heat treatment conditions after HIP process on microstructural refurbishment in cast nickel-based superalloy, GTD-111, High Temp. Mater. Processes, 2007; 26: [7] Wangyao P., Zrnik J., Mamuzic I., Polsilapa S. and Klaijumrang S., Restoration and thermal stability investigation of intermetllic phase in exposed nickel base superalloy Udimet 500 turbine blades, Metallurgija, 2007; 46: [8] Wangyao P., Polsilapa S., Chaishom P., Zrnik J., Homkrajai W. and Panich N., Gamma Prime Particle Coarsening Behavior at Elevated Temperatures in Cast Nickel Base Superalloy, GTD-111 EA, High Temp. Mater. Processes, 2008; 27: [9] Wangyao P., Kraus L., Zrnik J. and Nemecek S., Effect of deformation condition on structure development in nickel base alloy, J. Mater. Process. Technol, 2007; 192: [10] Sajjadi S.A., Nategh S. and Guthrie R.I.L., Study of microstructure and mechanical properties of high performance Ni-base superalloy GTD-111, Mater. Sci. Eng., A, 2002; 325: [11] Nategh S. and Sajjadi S.A., Dislocation network formation during creep in Ni-base superalloy GTD-111, Mater. Sci. Eng., A, 2003; 339: [12] Liburdi Engineering Limited, [13] Daleo J.A., Ellison H.A. and Boone D.H., Metallurgical considerations for life assessment and the safe refurbishment and requalification of gas turbine blades, J. Eng. Gas Turbines Power, 2002; 124:

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