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Keywords: Recrystallization (RX) defects formed in the gibbosities induced by platinum chaplet pins were studied by ex-
Single crystal periments and simulations for single crystal (SX) blade castings. Recrystallization occurs in 39 of the 80 gibb-
Recrystallization osities and can penetrate more than 250 μm into the SX blade. The RX occurrence ratios for the gibbosities in the
Platinum chaplet pin upper, middle and lower positions of the blade are 83%, 50%, and 8% respectively, indicating a strong sensi-
Gibbosity
tivity of RX to the location height of the gibbosity. The microstructure is SX without the presence of micro
FEM simulation
Superalloy
misoriented grains in the cross-section of gibbosity of as-cast sample. Secondary carbide particles are found at
the interface between the RX and SX grains. A composite image of backscattered electron (BE) and electron
backscatter diffraction (EBSD) shows that the migration of the RX interface is hindered by coarse eutectic
particles. A thermal elastoplastic model that considers the anisotropic mechanical properties of SX superalloys
and is coupled with a finite-element method (FEM) was utilized to predict the deformation behavior during
directional solidification. The FEM results reveal that the equivalent plastic strain (PEEQ) tends to concentrate in
the gibbosities, and this gives a reasonable and reliable explanation for RX formation.
1. Introduction are arranged on either side of a SX hollow blade to fix the core. Fig. 1(c)
presents the schematic diagram of Pt chaplet pin and the induced
Recrystallization (RX) defects can significantly influence the service gibbosity. The chaplet extends from the core, across the SX blade, to the
life of single crystal (SX) turbine blades and vanes in aero-engines. The inside of ceramic mould, and the gibbosity is formed on the surface of
new grain boundaries introduced by RX decrease the creep rupture the blade (red dashed line in Fig. 1(c)). This technique can significantly
resistance of Ni-based SX superalloy blades due to the lack of elements reduce the relevant defects induced by the core, such as core break-
that can strengthen the grain boundaries (Mathur et al., 2017). Plastic through and exposure (black circle in Fig. 1(a), the core penetrates the
strain is usually considered as the main reason for the occurrence of RX thin-wall of blade airfoil), and the rejection rate caused by these defects
in blade castings, and can originate during many processes such as decreases from 90% to less than 5%. However, the gibbosity formed in
solidification contraction, shell removal and sand blasting (Jo et al., the position of chaplet on the SX blade surface can be hindered by the
2003). In addition, the difference in thermal expansion coefficients ceramic mould during DS, thereby leading to the formation of shear
between superalloys and ceramic moulds is another important reason stress. This significantly increases the probability of RX, which can
why plastic strains can be induced during the cooling process. The decrease the mechanical properties of the SX blade (Ning et al., 2013).
nucleation of RX grains is usually driven by plastic strain along with the Porter and Ralph (1981) reported that RX nucleation was prone to
deformation energy stored during the manufacturing process; this type occur by subgrain coalescence, and the subsequent growth was attrib-
of RX is called static RX (Reyes et al., 2015). uted to strain-induced boundary migration of the grain boundary at
As the shapes of hollow airfoils with cooling channels become which RX nucleated. Zhuo et al. (2015) pointed out that the subgrain
progressively more complex, some specific technologies (e.g., chaplets boundaries formed in the SX matrix were transformed from the dis-
comprising platinum pins) are often used to meet the needs of pro- location walls that formed with the migration of dislocations during the
duction (Salkeld et al., 1995; Ning et al., 2013; Jago, 1996). During the annealing process. Mathur et al. (2017) reported another surface nu-
directional solidification (DS) process, the core is easily driven to shift cleation mode, in which the micro-grains of γ’ phase in surface eutectics
by the flowing molten alloy around it; therefore platinum chaplet pins could coarsen during solution heat treatment. Panwisawas et al. (2013)
are used to keep them stable. As shown in Fig. 1(a) and (b), 12 chaplets and Li et al. (2015b) proposed isotropic and anisotropic mechanical
⁎
Corresponding author.
E-mail address: scjxqy@tsinghua.edu.cn (Q. Xu).
https://doi.org/10.1016/j.jmatprotec.2018.04.036
Received 17 July 2017; Received in revised form 20 April 2018; Accepted 21 April 2018
Available online 22 April 2018
0924-0136/ © 2018 Elsevier B.V. All rights reserved.
R. Wang et al. Journal of Materials Processing Tech. 259 (2018) 169–179
Fig. 1. SX turbine blade with platinum chaplet pins and gibbosities: (a) front
and (b) back sides, (c) schematic diagram of a Pt chaplet pin and an induced Fig. 2. Positions of Pt chaplet pins and induced gibbosities on the surface of the
gibbosity. designed blade casting: (a) front and (b) back sides.
models to simulate the scale of plastic strain accumulated in SX castings cooling zone through a baffle at the constant rate of 5 mm/min. After
during the DS process, respectively. Zambaldi et al. (2007) simulated casting, the blades were subjected to the standard heat treatment (SHT)
the RX evolution around the indentation in SX superalloy by combining consisting of the solution and aging processes (Table 2), which is si-
the cellular automaton method and finite-element method (FEM) based milar to the process employed in commercial production.
on crystal plasticity theory. Rettberg and Pollock (2014) studied the To inspect the surface RX grains, a mixed chemical solution (50%
influence of localized RX on macroscopic creep rates and developed a hydrochloric acid and 50% hydrogen peroxide) was used for etching the
model for the prediction of RX-accelerated tertiary creep. Jo and Kim blade castings. After macro-etching, the macro RX areas can be easily
(2003) found that the surface RX in the SX CMSX-2 superalloy did not detected on a sample surface by optical inspection. When such a sample
reduce creep rupture life at 982 °C, 240 MPa owing to the strengthening is viewed under a directional light source, the RX areas are seen as local
effect of a surface oxide layer. The early initiation of surface cracks on chromatic aberrations, with different reflectivities indicating that they
grain boundaries normal to the applied stress implemented harmful differ in crystallographic orientation from the SX matrix. The number of
effects to the SX specimens, in accordance with the investigation of gibbosities (na, subscript a denotes gibbosity #a) that are recrystallized
Zhang et al. (2012). However, the influence of surface gibbosity on RX at each gibbosity position was counted to calculate the RX occurrence
behavior and the prediction of deformation in the gibbosity of blade rate at this position (na/12, 12 is the total number of gibbosities at each
casting were seldom reported. gibbosity position). In order to observe the RX microstructure, the
The present research focuses on the investigation of RX behavior in gibbosity positions were carefully cut down from the blade casting
blades with gibbosities on their surfaces. In this regard, a blade casting using electrical discharge machining (EDM) normal to the surface
with several gibbosities on its surface was designed, directionally soli- across the gibbosity peak. Subsequently, mechanical grinding and pol-
dified and heat-treated. The recrystallized gibbosities at various heights ishing were performed. The as-polished samples were etched using
were counted and characterized. The nucleation mechanism of the RX Marble’s reagent to enhance the contrast between the precipitate and
grains was discussed. To further study the driving force for nucleation matrix, then observed by optical microscopy (OM, Zeiss AM10 OM) and
and growth, a thermal elastoplastic model considering the anisotropic scanning electron microscopy (SEM, Merlin FEG-SEM). Composition
mechanical properties of SX superalloys was utilized to predict the measurements were performed using energy-dispersive spectroscopy
deformation behavior of blade castings during DS. (EDS). The samples for crystal orientation measurements were elec-
trochemically polished, and the images were captured in backscattered
2. Methods electron (BEI) and electron backscatter diffraction (EBSD) mode.
A model of a blade casting with five platinum chaplet pins and In classical theory, plastic strain, as the main driving force, has been
gibbosities was designed for a length of 99 mm that approximately widely used to explain the nucleation and growth of RX grains.
equals the length of an aero-engine turbine blade, as shown in Fig. 2. However, the exact temperature and time at which plastic strain occurs
Wax patterns were fabricated by an additive manufacturing technology, is difficult to measure experimentally. Therefore, it is necessary to use
and spiral grain selectors were added to the very base of them. Chaplets FEM and a constitutive model that considers the anisotropic mechanical
of platinum wire were inserted into the wax blades, and the gibbosities behavior of SX superalloys to calculate the equivalent plastic strain
formed around them. Four wax blade patterns were arranged in one (PEEQ) in blade castings during the DS process. Because the elastic and
cluster. In this study, three types of mould clusters with angles of 0°, 45° plastic strains are mainly caused by the difference in coefficients of
and 90° were fabricated (Fig. 3). The ceramic shells were produced by thermal expansion between the castings and the shells/cores during the
ceramic slurries and particles. The superalloy used in this study was a solidification process, the accuracy of PEEQ is dependent on that of
second-generation SX superalloy, DD6, whose nominal chemical com- temperature distribution. This distribution is extracted from the simu-
position is presented in Table 1. The SX blade castings were prepared in lation results of ProCAST and then imported to Abaqus as a pre-defined
an ALD industrial vacuum Bridgman furnace. The pouring temperature temperature field. Both ProCAST and Abaqus are commercially avail-
was 1550 °C. After preheating, pouring and heat preservation, the chill, able FEM software packages. To ensure accuracy of the temperature
ceramic shell and alloy were withdrawn from the heating zone into a field calculation, experimentally measured temperature/time-
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Fig. 3. Schematic of three mould clusters. Four blade patterns are arranged in one cluster at (a) 0°, (b) 45° and (c) 90° angles with respect to the radial direction.
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Table 3
Mechanical parameters used in the simulation (Li et al., 2015b).
Parameter 25 °C 700 °C 760 °C 850 °C 980 °C 1070 °C 1100 °C
E < 001 > (GPa) 131.5 107 105.5 98 80.5 69.5 67.5
μ < 001 > 0.344 0.374 0.377 0.383 0.390 0.399 0.413
G < 001 > (GPa) 142 93.6 98.3 71.2 85.4 75.7 66.6
K 6.2 3.47 3.44 2.46 1.87 2.15 2.36
L 3.1 1.74 1.72 1.23 0.94 1.08 1.18
∂f dλ
dε pl = dλ = b
∂σ f (11)
where b can be written as:
3.1. Macroscale recrystallized gibbosities The RX grain morphology in the cross-section of a gibbosity is
shown in Fig. 6 (a). The grain can be divided into two parts by the red
After macroscale chemical etching, the RX grains can be detected dashed line that represents the boundary between the SX blade and the
from the various reflectivities observed under light irradiation. As gibbosity: (1) the part inside the gibbosity (marked by the yellow line)
shown in Fig. 4, the samples annealed using SHT show large RX areas and (2) the part inside the SX blade (marked by the red line). The
on the gibbosity surface, including some twinning grains. However, former will be removed during the subsequent process of removal of the
almost no RX was observed at other locations on the blade surface. The gibbosity, while the latter will actually destroy the integrity of the SX
macroscale experimental results reveal a strong sensitivity of RX to the structure and reduce its mechanical properties.
gibbosity on the surface of a blade casting. The largest RX and twinning As shown in Fig. 6(a), a one-dimensional coordinate system was
grains almost cover the whole surface of the gibbosity, but cannot cover defined to describe the grain depth x. The origin of the coordinate
its round edge. (0 μm) is on the red dashed line (the boundary between the SX blade
The number of gibbosities with RX grains at five gibbosity positions and the gibbosity), and the value above zero represents that RX grains
in three mould clusters is summarized in Fig. 5. There are four identical have grown into the inside of the SX blade casting (left side of the red
blade castings arranged in one mould cluster, such that the maximum dashed line). The minimum and maximum depth of RX grains and the
number of recrystallized gibbosities at the same gibbosity position in total number of recrystallized gibbosities at five gibbosity positions are
one mould cluster is four. The location height of #3 (10 mm) is lower summarized in Fig. 7. Although RX occurred in nearly half of the
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Fig. 6. Structure morphology in the cross-section of gibbosity. (a) OM graphic. (b) Twinning RX grains by EBSD detection. The inset is a local magnified composite
image of backscattered electron (BE) and EBSD, showing the eutectic retarding the migration of the RX interface. (c) Eutectic particles at grain boundary.
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Fig. 9. Elemental segregation in region near the grain boundary between RX and SX matrix of as-heat-treated samples.
boundaries between SX matrix grain and mis-orientated RX grains decreases with the decrease of temperature. Hence, phases formed at
(Fig. 8(b)). Area scanning results of EDS measurement (Fig. 9) shows elevated temperature are likely to remain. The elements such as C and
that the contents of elements W, Mo and Re are extremely high in NPPs Hf are likely to accumulate in grain boundaries and play a role in grain
compared to the SX and RX regions. Thermodynamic calculation was boundary strengthening. Besides, the chemical composition close to the
conducted with Pandat software and PanNi database which is based on formation position of precipitated phase dose not conform to the
the experimental measurement. According to the calculation results, nominal chemical composition of DD6 superalloy, so the formation
the phases γ, γ’, M6C, M23C6 and μ can form in DD6 superalloy with condition of these phases does not completely conform to the calcula-
nominal chemical composition, but the atom activity gradually tion results. There are difference in chemical composition between M6C
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Fig. 10. SEM and EDS spectroscopy of the precipitated particles in grain boundary: (a) particle morphology, the particle for point EDS is marked at the upper left
corner; (b) the EDS spectroscopy of the marked precipitated particle.
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Fig. 12. Difference between temperature distribution of blade castings in (a) 0° and (b) 90° clusters. (c) The comparison of PEEQ evolution at gibbosity#1 in 0° and
90° clusters during solidification.
temperature, plastic strain will accumulate. This process is described in 3.4. Evolution of PEEQ
Fig. 12(c); the point chosen for comparison is the same position of
gibbosity #1 in the 0° and 90° clusters. As can be seen, there is a minor PEEQ represents the extent of plastic deformation and crystal slip,
difference in the evolution curves of the Hill potential function, leading which is essentially ascribed to the formation of dislocation. Zhuo et al.
to different yield behaviors, but the variation tendencies are similar. (2015) have observed that the dislocation can migrate to form the
Once the PEEQ accumulates, it is irreversible, and hence it is related to dislocation walls during annealing, and the SX matrix can be separated
the stress status of every moment. Different temperature distributions by these dislocation walls to provide the RX nucleation sites, which
lead to the differences in stress status in the three mould clusters. As a conforms with the traditional RX nucleation mode of dislocation in-
result, the PEEQ is influenced by the mould clusters. Fig. 13 indicates duction. On the macro scale, PEEQ can well represent the extent of
that although the simulated PEEQ varies with clusters, the stress status plastic deformation and slip. Owing to heterogeneity of the finite-ele-
and variation trend inside the blades are similar. For the semi-quanti- ment mesh, it is important to select reasonable mesh size to ensure
tative judgment of RX, it is completely acceptable as long as the trends calculation accuracy. In this study, coarse and fine meshes were allo-
and values are correct in a single cluster. Therefore, the 0° cluster, the cated to the simple blade body and complex geometric features, re-
results of which are closest to the average values of the three clusters, is spectively, to achieve an appropriate balance between computational
chosen for the following simulation. efficiency and accuracy, as shown in Fig. 14. When the temperature of
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Fig. 14. PEEQ distributions in blade casting when the temperature of gibbosity#1 (the uppermost gibbosity) decreases to 800 °C: (a) front side; (b) back side.
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Fig. 15. Evolution of PEEQ distribution in the cross-section of gibbosity#1 at (a) solidus 1342 °C, (b) 1200 °C, (c) 1000 °C and (d) 800 °C.
Fig. 17. Simulated A-PEEQ, B-PEEQ, T-PEEQ and PEEQ distributions on the (a)
(c)(e)(g)(i) surfaces and (b)(d)(f)(h)(j) cross-sections of five gibbosities at
800 °C.
Fig. 16. Variation of simulated PEEQ with the decrease in temperature at the
(a) top and (b) bottom parts of five gibbosities during solidification.
through the micro-grains of γ’ in the surface eutectic, concurrently in Fig. 18. PEEQ profile along the red line (upper-right inset) in the cross-section
the presence of moderate casting deformation (Mathur et al., 2017). of gibbosity#1. (For interpretation of the references to colour in this figure
The micro-grains in the latter nucleation mode resemble the freckle- legend, the reader is referred to the web version of this article).
chain defects of DS components, and it should be noted that significant
elemental segregation remains even after heat treatment, as demon- as concentration features that induce large mechanical deformation,
strated in the experimental results of Mathur et al. (2017). For the blade and the induced PEEQ is the driving force of RX nucleation and growth.
castings with gibbosities, the EDS maps of different elements in the
grain boundary between RX and SX grains are presented in Fig. 9. The 4. Conclusions
secondary carbide particles, enriched in Ta, W, Re and Co, appeared at
the grain boundary; however, almost no difference in the elemental Experiments and simulations were conducted to investigate the ef-
distribution was measured between the RX and SX regions. In addition, fect of gibbosities on RX formation in SX blade castings. Based on the
no misoriented grains were found in the surface and cross-sections of results obtained above, the following conclusions can be drawn:
as-cast gibbosities by OM and EBSD observations. Neither of these re-
sults conform to the characteristics of the latter nucleation mode. 1) 48% (29/60) of gibbosities exhibited RX grains after SHT (solution
Moreover, the FEM results reveal that the Pt pin and gibbosity here act and aging). Most RX grains exist inside the gibbosities, but some still
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penetrate the blades to a depth of 300 μm, damaging the integrity of Li, Z., Xiong, J., Xu, Q., Li, J., Liu, B., 2015b. Deformation and recrystallization of single
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