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Contribution of constitutional liquation of gamma prime precipitate to weld HAZ cracking of cast Inconel 738 superalloy
O.A. Ojo, N.L. Richards, M.C. Chaturvedi
*
Department of Mechanical and Industrial Engineering, University of Manitoba, Room 356, Engineering Building, Winnipeg, Manitoba, Canada R3T 5V6 Received 14 August 2003; received in revised form 17 November 2003; accepted 17 November 2003

Abstract The weld heat aected zone (HAZ) cracking in cast Inconel 738 superalloy has been examined. Constitutional liquation of the main strengthening phase of the alloy c0 , which is also present in signicant volume after pre-weld heat treatment, was found to contribute signicantly to grain boundary liquation and its attendant cracking in the HAZ. 2003 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
Keywords: Nickel alloys; Welding; Constitutional liquation; Superalloys; HAZ cracking

1. Introduction Inconel 738 is a precipitation-strengthened nickel base superalloy which is widely used in hot sections of gas turbine engines due to its excellent elevated temperature strength and superior hot corrosion resistance. It is strengthened primarily by precipitation of ordered L12 intermetallic Ni3 (Al,Ti) c0 phase. Inconel 738, like other precipitation hardened nickel base superalloys that contain substantial amount of Al and Ti (>6 wt.%), is generally considered very dicult to weld due to its high susceptibility to heat aected zone (HAZ) cracking during welding and post weld heat treatment by strain age cracking [1]. Cracking during welding of this alloy has been attributed mostly to large shrinkage stress occurring as a result of rapid precipitation of c0 particles during cooling from welding temperature [2]. However, it is known generally that weld cracking results from competition between mechanical driving force for cracking (stress/strain generation) and the materials intrinsic resistance to cracking. It has been found that liquation which could occur by dierent mechanisms, is the primary cause of low HAZ crack resistance in most austenitic alloys including precipitation hardened Ni base superalloys [3]. Combination of thermally induced
Corresponding author. Tel.: +1-204-474-6675; fax: +1-204-2616735. E-mail address: mchat@cc.umanitoba.ca (M.C. Chaturvedi).
*

welding strain and very low ductility in the alloy due to localized melting at grain boundaries results in HAZ liquation cracking. HAZ liquation is known to occur either by non-equilibrium interface melting below an alloys solidus or by equilibrium supersolidus melting. Subsolidus HAZ liquation which commonly occurs by constitutional liquation of second phase particles is generally considered more detrimental to crack resistance in that it extends the eective melting range of an alloy and also inuences the nature of supersolidus melting by pre-establishing non-equilibrium lm at a lower temperature which alters the reaction kinetics during subsequent heating [3]. This phenomenon which was rst proposed by Pepe and Savage [4] and has been observed by dierent investigators in various alloy system [57], occurs by a eutectic-type reaction between a second phase particle and the matrix producing a nonequilibrium solute rich lm at the particle/matrix interface. It has been reported that fully austenitic alloys that contain Nb and/or Ti can be highly susceptible to HAZ liquation cracking due to the formation of Nb and/or Ti rich low melting intergranular liquids [8]. Qian and Lippold [9] recently reported degradation in weldability due to grain boundary liquation in IN 718 resulting primarily from dissolution of Ni3 Nb d-phase and the associated Nb enrichment of grain boundary. Nevertheless, as fundamental as this liquation phenomenon is to HAZ cracking, very little information is available about its occurrence in Inconel 738 alloy. The above

1359-6462/$ - see front matter 2003 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved. doi:10.1016/j.scriptamat.2003.11.025

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results, coupled with the fact that Al and Ti (especially Ti, which also segregate into liquid in nickel base alloy) are melting point depressants, suggest that apart from the rapid precipitation eect of c0 phase on HAZ cracking, these c0 elements could also be contributing to high HAZ crack susceptibility in c0 precipitation-hardened alloy like Inconel 738 in other way. In the present study, constitutional liquation of MC carbides, boride, sulphocarbide, eutectic and coarse c0 precipitate was observed to have contributed to the HAZ liquation and its attendant cracking. Constitutional liquation of carbides, borides and suldes has been reasonably well discussed in other superalloy weldments [3,4,7], but constitutional liquation of c0 precipitates in any alloy system has not been reported in the literature. Convincing evidence of constitutional liquation of c0 phase was observed in this work and was found to be closely associated with the HAZ cracking. Considering the presence of signicant amount of c0 in the pre-weld solution treated condition (21%) and the fact that it is the prime strengthening phase of the alloy, observed liquation of c0 can have a very serious consequence on the weldability of IN 738. This communication reports the detection of constitutional liquation of c0 precipitate and discusses its contribution to HAZ cracking in Inconel 738 alloy.

quently etched electrolytically in 12 ml H3 PO4 + 40 ml HNO3 + 48 ml H2 SO4 solution at 6 V for 5 s. The microstructures of weld HAZ and thermally simulated samples were studied by optical and a scanning electron microscope equipped with energy-dispersive X-ray spectrometer.

3. Experimental results and discussion 3.1. Microstructure of as-cast, heat treated and welded materials The microstructure of the cast alloy essentially consists of extensive precipitation of ordered c0 intermetallic phase within the dendrite core and in the interdendritic region. Smaller volume fractions of various kinds of carbides/carbonitrides pre-dominantly MC type, boride, sulphocarbide and cc0 eutectic which form during ingot solidication are also present along the interdendritic region [11]. Formation of the non-equilibrium cc0 eutectic is due to microsegregation during ingot solidication [12,13]. The standard solution treatment at 1120 C for 2 h results in almost complete dissolution of primary c0 in the dendrite core with little, if any, dissolution of the particles in interdendritic region. The microstructure after this heat treatment consists of fairly regular coarse cuboidal, 0.60.8 lm size, primary c0 in the interdendritic region and ne (0.1 lm) spheroidal dispersion of secondary c0 , pre-dominantly in the dendrite core as well as within the interdendritic region (Fig. 1). The secondary c0 forms during cooling from the solution treatment temperature. The dendrite core is outlined by a ring of large c0 particles due to very rapid growth of these particles that contain higher Al and Ti content, immediately before solutioning. On overaging at 1025 C for 16 h both the primary and secondary c0 increased in size producing a microstructure consisting of bimodal distribution of large cuboids and smaller spheroids of size range 0.51 lm (Fig. 2).

2. Experimental procedures The cast alloy used in this study was Inconel 738 LC, with the following composition (wt.%) 0.11C, 15.84Cr, 8.5Co, 2.48W, 1.88Mo, 0.92Nb, 0.07Fe, 3.46Al, 3.47Ti, 1.69Ta, 0.04Zr, 0.012B balance nickel. 76.2 25.4 2.8 mm rectangular plates, on which a 1.3 mm deep V groove was machined, were given two dierent pre-weld heat treatments: (i) standard solution treatment at 1120 C for 2 h followed by argon quenching, (ii) solution treatment at 1120 C for 2 h and subsequent overaging at 1025 C for 16 h followed by water quenching. The latter is the heat treatment that has been developed to minimize weld cracking in IN 738 [10]. Heat treated samples were gas tungsten arc welded with IN 738 ller wire, using a current of 60 A DC and 10 V. The welding torch and wire speeds were maintained at 76 and 304 mm/min respectively. Cylindrical heat treated specimens of diameter 6 mm and length 115 mm were thermally cycled in a Gleeble 1500 thermomechanical simulation system by heating to 1140 and 1180 C at a rate of 150 C/s, held for 0.5 s and then quenched to room temperature in a jet of water. Welded specimens were sectioned transversely to the weld and the thermally cycled specimens were sectioned at the location of a spot welded thermocouple, which was used to control sample temperature. The sectioned samples were polished using standard metallographic techniques and were subse-

Fig. 1. Distribution of c0 in solution treated alloy.

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Fig. 4. Resolidied cc0 eutectic constituent from liquated c0 on cracked HAZ grain boundary. Fig. 2. Distribution of c0 in solution treated and aged alloy.

The disparity in dissolution behavior and size distribution of core and interdendritic c0 is a consequence of microsegregation that occurred during solidication of the alloy. Segregation, particularly of Ti into interdendritic regions resulted in higher c0 solvus and thus larger particle size after continuous cooling compared to particles in the core owing to precipitation occurring at a higher temperature. The solvus temperatures of interdendritic and core precipitates have been reported to be around 1170 and 1120 C respectively [12]. In addition to this distribution of c0 precipitate, discrete large c0 particles of average size of 1.8 lm were found along the grain boundaries of the two heat treated materials (Figs. 1 and 2). Microcracks of similar morphology were observed in welded samples that were pre-weld heat treated in the two dierent pre-weld heat treated conditions, with cracking occurring pre-dominantly in the HAZ in the regions slightly removed from the fusion boundary. The cracks displayed a relatively irregular and jagged path typical of liquation cracks, Fig. 3. Closer and careful examination of cracked regions at higher magnication by SEM revealed the presence of resolidication constituents with eutectic morphology that is characteristic of cc0 eutectic which formed at the later stage of solidication in this alloy. The resolidication constituents, which formed mostly on one side of the

cracks as shown in Fig. 4 for example, conrm formation of liquid lm on the grain boundaries in HAZ by liquation mechanism. Cracking occurred by decohesion across the solidliquid interfaces under the action of tensile welding stresses generated during cooling. 3.2. Constitutional liquation of c0 precipitate particles The basic requirement for the occurrence of constitutional liquation of an intermetallic compound Ax By in an alloy is the existence of Ax By particles at temperatures equal to or above their eutectic temperature on heating [4]. Consequently, the susceptibility of an Ax By type second phase to constitutional liquation in the weld HAZ must primarily be related to its solid state dissolution behavior, as complete dissolution prior to reaching the eutectic temperature will preclude the occurrence of liquation. The terminal eutectic temperature in Inconel 718 above which constitutional liquation of A2 B-type Laves phase and NbC particles were observed was found to correspond to the terminal reaction peak temperature during thermal analysis [7]. In Inconel 738, the temperature of cc0 eutectic reaction occurring towards the end of solidication process was determined by dierential thermal analysis to be around 1198 C [13], though Rosenthal and West [12] later reported that the eutectic reaction takes place over a range of temperature which could be as low as below 1180 C. What is evident is that the cc0 eutectic temperature is below 1200 C in this alloy, which is below the quoted equilibrium solidus temperature of IN 738, which is around 1232 C. During welding, dissolution behavior of c0 precipitates is expected to deviate from equilibrium due to rapid thermal cycling involved. An attempt has been made to model particle dissolution under rapid heating condition by an analytical technique as well as through the additivity and isokinetic approach [14]. The results of the two methods, which were found to be in good agreement with numerical dissolution model and experimental results, show that the degree of particle

Fig. 3. Crack due to liquation of c0 .

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dissolution depends on interplay between the heating rate and the initial particle size. Soucail and Bienvenu [15] in separate work, studied solid state dissolution of the c0 phase in Astroloy superalloy at equilibrium and under rapid heating. Their results, which are in agreement with those of Bjorneklett et al. [14] showed that there is a signicant departure from equilibrium under rapid heating condition, in that the temperature of complete solid state dissolution increased with increasing heating rate and this departure is dependent on the initial particle size. This increase in complete dissolution temperature was found to be more pronounced with increase in particle size. An increase of about 120 C in complete dissolution temperature was reported for c0 precipitates with initial size of 0.8 lm under a heating rate of 8 C/s. In fusion welding process, like the one used in the present work, typical heating rate normally exceeds 150 C/s and as such, variations in c0 dissolution behavior of c0 particles can be expected to depend on the particles location and size, with the possibility of some coarse particles remaining undissolved above 1200 C resulting in their constitutional liquation. It may be argued that liquation of intergranular c0 particles cannot be used to conclude the occurrence of constitutional liquation of the precipitate, considering that other liquation mechanisms may also be operative at grain boundaries, such as constitutional liquation of MC type carbides and possibly liquation due to segregation of low melting point depressing elements like boron. Consequently intragranular particles located up to 15 lm away from HAZ grain boundaries and distinctly separated from other liquating phases were closely examined. Evidence of c=c0 interface liquation was observed not only along the grain boundaries but more importantly within the grains of the HAZ (Figs. 35). The solute rich liquid pool adjacent to liquating particles is expected to commence solidication rst as gamma and then on reaching the eutectic temperature transform to cc0 eutectic product. On further cooling, c0 could precipitate out of the newly formed supersaturated c phase resulting in a resolidied region consisting of coarser c0 precipitate versus adjacent unmelted matrix

and ne cc0 eutectic protruding into the last area to solidify. The microstructure that forms depends on the volume and composition of liquid present at the peak temperature. These two types of resolidied morphology were observed in this work with the intragranular particles having ne resolidied structure. High magnication SEM image (Fig. 5) suggests that some of these resolidied regions contain ne cc0 eutectic which formed at the terminal stage of the solidication process. This suggestion was further supported in instances where a complete liquation of the intragranular precipitates occurred. Fine cc0 eutectic colonies were oriented with their crown region protruding into the last liquid to solidify, which is the typical mode of cc0 eutectic formation [16]. An additional indication of c=c0 interface melting is the observation of what appears to be voids or cavities in the immediate vicinity of extensively liquated intraganular particles (Fig. 5). It is known that voids and cavities often form in melted and resolidied regions in superalloys owing to the expansion and contraction accompanying solidication. Similarly, microstructural examination showed evidence of liquation at the interfaces of intragranular c0 particles of a sample rapidly heated to 1180 C as compared to a sample heated to lower peak temperature of 1140 C using a Gleeble simulation system (Figs. 6 and 7). It is to be noted that atom probe eld ion microscopy (APFIM) study of nickel base superalloys showed that there was no boron segregation to the interfaces of intragranular c0 particles [17]. Consequently, the occurrence of a liquid lm surrounding the intragranular c0 precipitates which are away from other liquating phases can only be reasonably attributed to constitutional liquation of the intermetallic particles [4]. It was observed that the closer these particles were to the fusion line, that is increased peak temperature, the more pronounced the liquation. This indicates that the coarse particles, that did not completely dissolve before reaching the eutectic temperature, constitutionally liquated, with the extent of liquation increasing with the

Fig. 5. Liquation of intragranular c0 precipitate in the weld HAZ.

Fig. 6. Liquation of intragranular c0 precipitates in Gleeble simulated sample at 1180 C (water quench).

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Fig. 7. Intragranular c0 precipitates in Gleeble simulated sample at 1140 C (water quench).

increase in peak temperature experienced in the HAZ i.e. regions closer to the fusion boundary.

4. Eect of constitutional liquation of c0 particles It has been recognized in many studies on HAZ cracking that the mere occurrence of liquation is not sucient to produce a crack susceptible microstructure. Susceptibility to cracking depends on penetration and wetting of grain boundary, liquid lm thickness and its stability to temperatures at which sucient thermal and mechanical stresses are generated on cooling. Wetting of a grain boundary is enhanced if the solidliquid interfacial energy is small compared to the grain boundary energy. Considering that the metastable liquid produced by constitutional liquation always reacts with the solid through solute back diusion, the non-equilibrium solidliquid interface energy is very low [18] and as such extensive grain boundary penetration and wetting by lm produced by constitutional liquation of c0 particles is expected. This was observed in all the samples with signicant penetration and spreading of the lm along the grain boundary (Fig. 8), even to the lower temperature subsolidus region of the HAZ. Interaction of the lm with grain boundary segregated surface active ele-

ments like boron could also aid the wetting behavior, as boron rich phase was observed as part of the resolidication constituents along some uncracked grain boundaries. Furthermore, as can be seen from the following expression [19], r 2cL =h (where r is the tensile stress required to overcome surface tension cL on a boundary containing liquid lm of thickness h), any parameter which contributes to an increase in the grain boundary lm thickness h, would reduce the crack resistance. The high volume fraction of liquating c0 and the large grain size of the cast alloy (500800 lm) are factors that could increase lm thickness and thus make the cast IN 738 alloy more susceptible to weld cracking. Liquid lm penetration from constitutionally liquated c0 particles in adjacent grains and close to the grain boundaries were found to contribute to intergranular liquation (Fig. 8). In terms of lm stability to lower temperatures, this can be assessed by considering subsolidus portion of the HAZ. The result of Gleeble thermal simulation showed that considerable c0 liquation is occurring as low as 1180 C. In this HAZ region, complete liquation of coarse particles may not be realized during the time the specimen remains at peak temperature during welding. On cooling, the low diusivity of Ti in the surrounding austenite matrix and its low partition coecient (0.6) could enable the existing liquid to persist to a much lower eutectic temperature, thereby increasing the local eective solidication range which would reduce the crack resistance. It should be mentioned that the cc0 eutectics in the alloy which were formed during ingot solidication and also observed to liquate in the HAZ, are a non-equilibrium solidication product and as such can be removed by appropriate preweld thermal treatment. In contrast, however, the c0 precipitates are an essential strengthening phase which are considered better to be in coarsened form in preweld material to induce enhanced ductility in the material for relieving welding strains. The detection of constitutional liquation of c0 precipitates in this alloy is considered crucial and signicant due to its inevitable presence as the main strengthening phase, high volume fraction and the lower eutectic temperature relative to the alloys equilibrium solidus. It is thus suggested that in addition to the eect of rapid on-cooling precipitation of c0 on HAZ cracking, the occurrence of constitutional liquation of c0 precipitate could as well be another contributing factor to the high HAZ crack susceptibility of this and other precipitation strengthened nickel base superalloys containing high volume fraction of c0 precipitate.

5. Summary and conclusions

Fig. 8. Liquid lm from liquated c=c0 interface of intragranular particles can be observed penetrating HAZ grain boundary.

1. Resolidied constituents were observed along cracked grain boundaries in the HAZ of welded cast

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IN 738 alloy and it is concluded that one of the factors responsible for HAZ cracking in this alloy is grain boundary liquation. 2. Constitutional liquation of both intragranular and intergranular c0 precipitates was found to be contributing signicantly to the HAZ liquation. 3. Liquid lms from liquated c0 precipitates were observed to exhibit extensive penetration and wetting of grain boundaries even to the lower temperature subsolidus region of the HAZ. 4. Constitutional liquation of c0 precipitates could as well be a contributing factor to the high HAZ crack susceptibility of other precipitation hardened nickel base superalloys with high volume fraction of c0 precipitate particles. Acknowledgements The authors would like to thank the consortium of Manitoba aerospace industries and NSERC for the nancial support. One of the authors (OAO) also acknowledges gratefully the award of Graduate Fellowship from NSERC and the University of Manitoba.

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