Intermetallics 18 (2010) 13791384

Contents lists available at ScienceDirect

Intermetallics
journal homepage: www.elsevier.com/locate/intermet

Mechanical properties of a forged Fe25Al2Ta steam turbine blade

P. Hanus a, b, *, E. Bartsch a, M. Palm a, R. Krein c, K. Bauer-Partenheimer d, P. Janschek d
a

r Eisenforschung GmbH, Max-Planck-Strasse 1, D-40237 Du sseldorf, Germany Max-Planck-Institut fu Technical University of Liberec, Studentska 2, Liberec 461 17, Czech Republic c now at: Salzgitter Mannesmann Forschung GmbH, Ehinger Str. 200, D-47259 Duisburg, Germany d Leistritz Turbinenkomponenten Remscheid GmbH, Lempstrasse 24, D-42859 Remscheid, Germany
b

a r t i c l e i n f o
Article history: Received 11 October 2009 Received in revised form 30 November 2009 Accepted 29 December 2009 Available online 25 January 2010 Keywords: A. Iron aluminides, based on Fe3Al B. Mechanical properties at high temperatures B. Creep (properties and mechanisms) B. Microstructure B. Yield stress

a b s t r a c t
The mechanical properties of samples taken from different parts of a 650 mm long steam turbine blade forged from Fe25Al2Ta (in at.%) by conventional forging on a counterblow hammer were examined. The hardness, brittle-to-ductile transition temperatures (BDTT), the yield stress in compression and in tension, and the creep behaviour were studied and compared with the same material in the as-cast and heat-treated state. Though forging apparently improves the mechanical properties they are still not optimal because of a too large grain size which stems from the insufciently rened microstructure in the cast precursors. Because some distinct features were observed during creep testing, microstructures of crept samples were investigated by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). These investigations revealed that the increased creep resistance below 700  C is caused by crystallographically oriented sub-micron sized precipitates of a Heusler phase. 2010 Elsevier Ltd. All rights reserved.

1. Introduction Fe3Al-type iron aluminides have been studied widely as candidates for high-temperature structural applications [13]. Their excellent corrosion resistance, promising wear resistance, and low density qualify them to replace Fe-based materials and stainless steels [4]. However, their ductility at low temperatures and creep strength at high temperatures have to be improved. To this end numerous investigations have been carried out. For strengthening at high temperatures incoherent precipitates such as other intermetallic phases, carbides, borides, coherent precipitates, or increasing the order of the matrix have been employed [510]. For enhancing ductility thermomechanical processing such as hot extrusion, rolling and forging have been tested [1115]. Currently work on Fe25AlxTi and Fe25AlxTa (compositions always in at % except noted otherwise) alloys was started [1618] which led to forging of large steam turbine blades [19]. The present paper reports on the microstructures and mechanical properties of specimens taken from different parts of a forged steam turbine blade.

2. Experimental An alloy of the composition Fe25Al2Ta (at.%) was produced by vacuum induction melting (VIM) and cast into a cold copper mould. Steam turbine blades were forged from the castings on a counterblow hammer at about 1100  C using standard tooling otherwise used for forging of 912 wt.% Cr steels (for details see [19]). Samples were cut from the root (R in Fig. 1) and the bottom (A), the middle (B), and the tip (C) of the airfoil by electrical discharge machining (EDM). The microstructures were studied by light optical microscopy (LOM) and scanning electron microscopy (SEM) using JEOL 6400, JXA-8100, and Hitachi S-530 instruments. A transmission electron microscope (TEM) Phillips CM20 operated at 200 kV and equipped with an energy-dispersive spectrometer (EDS) was used to identify tiny particles that formed in crept samples. Thin foils for TEM were prepared by electro polishing at 30  C in a solution of 30 vol.% HNO3 and 70 vol.% of methanol. The hardness and microhardness were determined using a Vickers indenter and a load of 500 g (HV/0.5) and 100 g (HV/0.1), respectively. The temperature dependent stress-strain behaviour was determined by compression tests in air at a strain rate of 104 s1 within the temperature range RT 1000  C for specimens from R and A and within RT 900  C for specimens from B. A few tensile test samples with a gauge length 32 mm and

* Corresponding author at: Technical University of Liberec, Studentska 2, Liberec 461 17, Czech Republic. Tel.: 420485353136; fax: 420485353631. E-mail address: pavel.hanus@tul.cz (P. Hanus). 0966-9795/$ see front matter 2010 Elsevier Ltd. All rights reserved. doi:10.1016/j.intermet.2009.12.035

1380

P. Hanus et al. / Intermetallics 18 (2010) 13791384

Fig. 1. Forged steam turbine blade [19]. The letters indicate the positions where samples for mechanical testing have been cut out of the blade.

a cross-sectional area of 3.5 5 mm2 were cut from parts R and A an tested in air between RT and 800  C at a constant deformation rate of 104 s1. For 4-point bending tests specimens with dimensions of 3 6 18 mm3 were cut along the length of the blade and were subsequently polished. Tests were carried out on specimens from parts R and A at a constant strain rate of 104 s1 between 400 and 800  C in air. The BDTT is taken as the temperature where the fracture strain increases from about 1% or less (referring to the outer bre) to 3% or more [20]. Creep samples from parts R, A and B with dimensions of 5 5 10 mm3 were tested in compression in air between 600  C and 750  C by step-wise increasing the load. 3. Results and discussion 3.1. Microstructure and hardness of the forged blade Microstructures of all parts of the forged blade are characterised by large (1001000 mm), elongated FeAl grains [19] (a more detailed analysis of the FeAl grains is obtained from the TEM observations reported below). The microstructure has only partially recrystallised during forging due to the pinning of the grain boundaries by ne precipitates of a hexagonal C14-type Laves phase [19]. The hardness evaluated from specimens taken from inside the blade is about 335 HV/0.5 and does not vary markedly within the different parts of the blade. However, samples taken from the surface of part C show some amount of surface hardening where the microhardness is 355 15 HV/0.1 at the upper (hammer) side and 376 9 HV/0.1 at the bottom (die) side. 3.2. Mechanical properties The ductility of the material has been characterised through 4-point bending tests carried out between 400 and 800  C and the results are compared with data which have been measured previously for the same alloy in the as-cast state (AC) and after a heat treatment at 1000  C for 200 h (HT) [17] (Fig. 2). It had been shown previously that ductility could be enhanced through a heat treatment by rening the microstructure, i.e. the heat-treated alloy had a smaller grain size than the as-cast alloy [17]. The BDTT of the AC material is about 750  C while in the HT state the BDTT is lowered to about 525  C. The BDTTs evaluated for the present material are 650  C for the root (R) and 525  C for the bottom of the airfoil (A). Apparently the somewhat smaller grain size and possibly a higher deformation during forging at the bottom of the airfoil led to the lower BDTT of A. The 0.2% compressive yield strength (s0.2) was evaluated on samples from parts R, A and B in the temperature range 201000  C

Fig. 2. Fracture strains (referred to the outer bre) determined from 4-point bending tests of samples of parts A and R of the forged blade. Data for the same alloy in the ascast (AC) and heat-treated 1000  C/200 h (HT) state are shown for comparison [17]. Arrows indicate fracture strains of more than 3% which can not be measured due to limitations by the experimental set up. Brittle-to-ductile transition temperatures (BDTT) are indicated by vertical lines.

and the results are again compared with the material in the AC and HT state (Fig. 3) [17]. The values for s0.2 for parts R, A and B are all above 100 MPa at possible application temperatures of 650750  C. However, compared with the AC and HT state values are considerably lower in all parts of the forged blade over the entire temperature range. Samples from parts R and A were also tested in tension. Due to their premature failure at lower temperatures the s0.2 yield strength could not be determined for all samples. While data for 600 and 800  C for R and A are comparable to values determined in compression, values for A are higher at lower temperatures. However, this is not attributed to a higher strength but to the premature failure of the samples. Apparently, samples of R failed at a lower load as R has a lower ductility than A as revealed by the 4-point bending tests. The data of the compressive creep tests between 600 and 750  C for samples from parts R, A and B are summarised in Fig. 4ad and are compared with data for the material in the AC and HT state [21,22] and with data for P92 [23], a 9 wt.%. Cr steel strengthened by

Fig. 3. Temperature dependence of the compressive yield stress s0.2 of samples from parts R, A, and B in comparison to the as-cast (AC) and heat-treated (HT) alloy [17].

P. Hanus et al. / Intermetallics 18 (2010) 13791384

1381

Fig. 4. Secondary creep rates at 600 (a), 650 (b), 700 (c) and 750  C (d) determined in compression by step-wise increasing the load of samples taken from parts R, A, and B. Data for the as-cast (AC) and heat-treated material (HT) for 650750  C [21,22] and for P92 at 650  C [23] are shown for comparison.

ne carbide precipitates, which is presently one of the most advanced materials for steam turbine applications. In the forged blade the creep strength is about the same in all tested parts, though data from part B are usually on the low side. The data also level those of the material in the as-cast state (AC) while the material shows higher creep strength after a heat treatment (HT). However, the creep strength in all parts of the forged blade is considerably higher at 650  C than that of P92 (Fig. 4b). It is noted that several sets of data show a marked change in the slope which is related to a change in the microstructure as will be discussed below. From Nortons power law [24] values for the stress exponent n have been derived (Table 1). For the forged material stress exponents of about 35 are observed at 700 and 750  C while at lower temperatures considerably higher stress exponents of about 1215 are found. This corresponds to stress exponents found for the AC

Table 1 Stress exponents n in Nortons power law [24] evaluated from the slopes of the double-logarithmic plots in Fig. 4. Some alloys exhibit a higher stress exponent at the beginning of the tests due to changes in the microstructure (n1; see text for detail). Data for the as-cast (AC) and heat-treated material are shown for comparison [21,22]. 600  C R A B HT AC 12.4 10.9 12.3 650  C n1 22.2 12.5 n1 28.6 14.9 11.4 14.4 14.4 700  C n1 10.8 5.1 n1 12.7 5.2 4.8 5.8 7.9 750  C 2.6 2.7 3.3 4.7 5.9

1382

P. Hanus et al. / Intermetallics 18 (2010) 13791384

and HT material which also show a much higher stress exponent below 700  C. The lower values are typical for FeAl-based alloys which are solid solution hardened while the higher values indicate strengthening by ne precipitates [10]. As noted above, some of the curves show a sudden change in the slope in that a higher stress exponent is observed at low strain rates while a lower stress exponent is observed at high strain rates. Such sudden changes in the stress exponent have been described before for FeAl-based alloys and have been attributed to changes in the microstructure [2527]. 3.3. Microstructure after creep In order to establish why the stress exponent changes markedly between 650 and 700  C and if the change in the slope of the creep curves is caused by a change in the microstructure SEM and TEM investigations were carried out. Fig. 5 shows the microstructure of part A after forging (Fig. 5a) and after creep at 650 (Fig. 5b) and 750  C (Fig. 5c). After forging the FeAl grains have partially recrystallised. In addition small precipitates are predominantly found at the FeAl grain boundaries, which have been identied as Laves phase by electron-probe microanalysis (EPMA) [19]. After creep at 750  C a comparable microstructure is observed in that large FeAl grains are observed which are separated by lines of elongated Laves phase precipitates which are several microns long (Fig. 5c). In contrast, only few Laves phase precipitates are observed after creep at 650  C. Instead, numerous oriented precipitates became visible inside the FeAl matrix at higher magnication (Fig. 5b). Because they were too small to identify them in the SEM, TEM observations on the sample crept at 650  C were performed. The TEM bright-eld (BF) micrograph in Fig. 6a shows a large particle that was identied by TEM-EDS as Laves phase and a FeAl matrix which contains numerous small precipitates. The dark-eld (DF) TEM micrograph of the FeAl matrix taken with the (100)B2/ (200)D03-superlattice reection (Fig. 6b) reveals the presence of B2-type anti-phase boundaries (APBs) and also shows ne precipitates which contain numerous fringes. Fig. 6c is a TEM BF micrograph which shows the ne precipitates within the FeAl matrix in higher magnication. The precipitates have a size of 50100 nm and frequently form small chains. An identication of the ne precipitates by selected area diffraction (SAD) on the employed TEM is rather complicated due to the small size of the particles. Even by employing the smallest aperture additional diffraction spots from the matrix cannot be avoided and these superimpose those of the precipitates, already indicating a close crystallographic relationship of the crystal structures of the precipitates and the matrix. However, the precipitates give a bright contrast in TEM DF taken with (111)D03-superlattice reection (Fig. 6d) and TEM-EDS showed that the particles have a much higher Ta content than the FeAl matrix. It is therefore concluded that the precipitates are the Heusler phase which has the L21 structure, which is the ternary equivalent to the binary D03 structure. The precipitates have formed on the (001) plains of the FeAl matrix and the chains of the particles are parallel to the <001> direction of the matrix. The same ne particles were identied by SEM and X-ray diffraction after creep at 650  C of the material in the HT state [21]. It is noted that Fig. 6d also shows the presence of numerous D03-type APBs which stem from the B2 4 D03 transition during cooling which takes place at 594  C in the present alloy [17]. The above observations comply perfectly with results previously obtained for Fe25Al2Nb [28,29]. After aging at or below 650  C TEM observations revealed the presence of ne coherent precipitates within the FeAl matrix which are characterised by numerous fringes. By examination with an analytical electron microscope (AEM) in SAD and convergent beam diffraction (CBED) mode the

Fig. 5. SEM micrographs with back-scattered electron (BSE) contrast of part A after forging (a) and after creep testing at 650  C (b) and 750  C (c). Within the FeAl matrix the white precipitates are Laves phase in a) and c) and Heusler phase in b).

particles were identied as L21 Heusler phase. The particles (p) are coherent with the matrix (m) and their orientation relationship was established as ({001}p//{001}m:<100 > p//<100 > m) [28]. When annealed for short times at 700750  C these precipitates were also observed but they transformed to C14 Laves phase after longer aging times [29]. The formation of the crystallographically oriented, sub-micron sized L21 precipitates below 700  C should explain the high stress

P. Hanus et al. / Intermetallics 18 (2010) 13791384

1383

Fig. 6. TEM micrographs of the sample from part A after creep at 650  C; a) bright-eld (BF) micrograph showing a large (dark) Laves phase particle and the FeAl matrix with numerous small precipitates (black); b) dark-eld (DF (100)B2/(200D03) near [001] matrix orientation) micrograph of the FeAl matrix showing B2-type anti-phase boundaries (APBs) and ne precipitates containing numerous fringes; c) BF micrograph showing chains of small particles (dark) within the FeAl matrix; d) DF (111)D03 micrograph of the same area as in Fig. 6c which also shows the presence of numerous D03-type APBs.

exponents that are observed at 600 and 650  C for all parts of the forged blade and also for the material in the AC and HT state (Table 1). At 700 and 750  C Laves phase precipitates are observed instead. They are considerably larger than the crystallographically oriented L21 precipitates and arranged in lines which are separated from each other by several hundred microns. Therefore these precipitates do not have a pronounced strengthening effect and therefore the stress exponents observed at 700 and 750  C are considerably lower than those at lower temperatures. The changes in the slope of certain creep curves, e.g. for part A at 650  C, may also be attributed to the change in the microstructure when the L21 Heusler phase starts precipitating on expense of the Laves phase. 4. Summary and conclusions The mechanical properties of different parts of a forged steam turbine blade were evaluated and they were compared with data measured previously for the same Fe25Al2Ta alloy in the as-cast (AC) and heat-treated (HT) state. The mechanical properties in general match those of the AC material but especially the yield strength and the creep strength are lower in all parts of the blade than for the HT material. These inferior properties are related to a non optimum microstructure as the forged material is still very coarse grained. This coarse microstructure stems already from the casting of the precursors and it has only partially recrystallised during forging because of pinning of the grain boundaries by Laves

phase precipitates. However, it can be concluded that forging improves the properties because parts that were more recrystallised showed a lower BDTT and a higher maximum yield stress in tension at lower temperatures. The creep tests showed two striking features in that the stress exponent n increased markedly below 700  C and that a sudden change in the slope in some of the curves was observed indicating again a marked change in the stress exponent during testing at certain temperatures. TEM investigations revealed that both effects are due to drastic changes in the microstructure. They also revealed for the rst time that the increased creep resistance in Fe25Al2Ta below 700  C is caused by sub-micron sized precipitates of a Heusler phase which are aligned in small chains along the <001> direction of the FeAl matrix. Acknowledgements The authors wish to thank Gerhard Bialkowski for EDM and mechanical testing and Nico Engberding for SEM observations. P.H. gratefully acknowledges nancial support by the Grant Agency of the Czech Republic through grant No. 106/08/P005. References
[1] Sauthoff G. Intermetallics. Weinheim: Wiley-VCH; 1995. p. 1. [2] Deevi SC, Sikka VK. Nickel and iron aluminides: an overview on properties, processing, and applications. Intermetallics 1996;4:35775.

1384

P. Hanus et al. / Intermetallics 18 (2010) 13791384 [17] Risanti DD, Sauthoff G. Strengthening of iron aluminide alloys by atomic ordering and Laves phase precipitation for high-temperature applications. Intermetallics 2005;13:131321. [18] Risanti DD, Sauthoff G. Ironaluminium-base alloys with strengthening Laves phase for structural applications at high temperatures. Mat Sci Forum 2005;865:4759. [19] Janschek P, Bauer-Partenheimer K, Krein R, Hanus P, Palm M. Forging of steam turbine blades with an Fe3Al-based alloy. Mat Res Soc Symp Proc 2009;1128:4752. [20] Risanti D, Deges J, Falat L, Kobayashi S, Konrad J, Palm M, et al. Dependence of the brittle-to-ductile transition temperature (BDTT) on the Al content of Fe-Al alloys. Intermetallics 2005;13:133742. [21] Palm M, Krein R, Milenkovic S, Sauthoff G, Risanti D, Stallybrass C, et al. Strengthening mechanisms for Fe-Al-based alloys with increased creep resistance at high temperatures. Mat Res Soc Symp Proc 2007;980:II0101. [22] Risanti DD. unpublished results. [23] Knezevic V, Sauthoff G, Vilk J, Inden G, Schneider A, Agamennone R, et al. Martensitic/feritic super heat-resistant 650 C steels design and testing of model alloys. ISIJ Int 2002;42:150514. [24] Nazmy MY. Creep. In: Stoloff NS, Sikka VK, editors. Physical metallurgy and processing of intermetallic compounds. New York: Chapman & Hall; 1996. p. 95125. [25] Whittenberger JD, Nathal MV, Gaydosh DJ. Compressive and tensile creep in Fe40Al0.1Zr0.4B at 1100 K. Intermetallics 1994;2:193200. [26] Krein R, Schneider A, Sauthoff G, Frommeyer G. Microstructure and mechanical properties of Fe3Al-based alloys with strengthening boride precipitates. Intermetallics 2007;15:117282. [27] Krein R, Palm M, Heilmaier M. Characterisation of microstructures, mechanical properties, and oxidation behaviour of coherent A2 L21 FeAlTi alloys. JMR 2009;24:341221. [28] Dimiduk DM, Mendiratta MG, Banerjee D, Lipsitt HA. A structural study of ordered precipitates in an ordered matrix within the FeAlNb system. Acta Metall 1988;36:294758. [29] Morris DG, Requejo LM, Munoz-Morris MA. A study of precipitation in D03 ordered FeAlNb alloy. Interemtallics 2005;13:86271.

[3] Stoloff NS. Iron aluminides: present status and future prospects. Mater Sci Eng 1998;258A:114. [4] McKamey CG. Iron aluminides. In: Stoloff NS, Sikka VK, editors. Physical metallurgy and processing of intermetallic compounds. New York: Chapman & Hall; 1996. p. 35191. [5] Mendiratta MG, Ehlers SK, Dimiduk DM, Kerr WR, Mazdiyasni S, Lipsitt HA. A review of recent developments in iron aluminides. Mat Res Soc Symp Proc 1987;81:393404. [6] Morris DG, Morris MA. Strengthening at intermediate temperatures in iron aluminides. Mater Sci Eng 1997;A239-240:2338. [7] Morris DG. Possibilities for high-temperature strengthening in iron aluminides. Intermetallics 1998;6:7538. [8] Bahadur A. Enhancement of high temperature strength and room temperature ductility of iron aluminides by alloying. Mat Sci Technol 2003;19: 162734. [9] Palm M. Concepts derived from phase diagram studies for the strengthening of FeAl-based alloys. Intermetallics 2005;13:128695. oz-Morris MA. Development of creep-resistant iron alumi[10] Morris DG, Mun nides. Mater Sci Eng 2007;A462:4552. [11] Flores O, Juarez J, Campillo B, Martinez L, Schneibel HJ. Forging of FeAl intermetallic compounds. San Francisco CA: Metallurgical Society Annual Meeting; 1994. 27.02.-03.0318. [12] Huang YD, Yang WY, Sun ZQ. Improvement of room temperature tensile properties for Fe3Al-based alloys by thermomechanical and annealing processes. Mater Sci Eng 1999;A263:7584. [13] Yu XQ, Sun YS. Hot working of Fe3Al based alloys. Mat Sci Technol 2004;20:33942. [14] Konrad J, Zeafferer S, Schneider A, Frommeyer G, Raabe D. Thermomechanical treatment of a Fe3Al alloy. Mat Res Soc Symp Proc 2005;842:416. [15] Kobayashi S, Takei A, Takasugi T. Grain renement for strengthening in Fe3Albased alloys through thermomechanical processing. Mat Res Soc Symp Proc 2009;1128:538. [16] Krein R, Palm M. The inuence of Cr and B additions on the mechanical properties and oxidation behaviour of L21-ordered FeAlTi-based alloys at high temperatures. Acta Mat 2008;56:24005.