Materials and Design 196 (2020) 109138

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Materials and Design

journal homepage: www.elsevier.com/locate/matdes

Sliver defect formation in single crystal Ni-based superalloy castings

Wenliang Xu a,1, Fu Wang a,b,⁎,1, Dexin Ma b, Xintao Zhu b, Dichen Li a, Andreas Bührig-Polaczek b
a
State Key Laboratory for Manufacturing System Engineering, School of Mechanical Engineering, Xi'an Jiaotong University, Xi'an 710049, China
b
Foundry Institute, RWTH Aachen University, Aachen 52072, Germany

H I G H L I G H T S G R A P H I C A L A B S T R A C T

• During directional solidification of SX

castings, dendrite fragmentation arose
the formation of sliver defect.
• The macroscopic and microscopic non-
uniform stress played significant roles
in the dendrite fragmentation.
• The possible solid fraction range for
fragmentation was suggested to be
0.6–0.8.
• The sliver occurrence may be correlated
to the formation of converging interface
between dendrite tips and mold wall.

a r t i c l e i n f o a b s t r a c t

Article history: Sliver is a typical grain defect in single crystal Ni-based superalloy castings produced by Bridgman directional so-
Received 27 July 2020 lidification. However, its formation mechanism has yet to be fully understood. In this study, the formation of
Received in revised form 2 September 2020 sliver defects was investigated with respect to the defect morphological features, the microstructure of defect ini-
Accepted 8 September 2020
tiation points, and the solidification conditions. Experiment results showed that sliver defects were originated
Available online 9 September 2020
from fragmentation of dendrite trunks and could developed to various morphologies. The misorientation range
Keywords:
of sliver grains was between 3.2° to 12°. Microstructural analysis results indicated that the dendrites fragmented
Single crystal Ni-based superalloys abruptly without significant plastic deformation. And the dendrite fragmentation could be facilitated by oxide in-
Directional solidification clusions and solidification pores. It was also found that the sliver defects were prone to occur at the interface
Dendritic solidification where primary dendrite converge to the mold inner wall. Based on the low misorientation level of sliver grains
Sliver defect in the experimental observation, the critical solid volume fraction range for fragmentation was suggested to be
0.6–0.8. The dendrite fragmentation was attributed to the non-uniform stress distribution in dendrite during so-
lidification. In addition, the effect of airfoil geometry of a typical blade casting and defect prevention methodology
were discussed.
© 2020 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND license (http://
creativecommons.org/licenses/by-nc-nd/4.0/).

1. Introduction

Single crystal (SX) Ni-based superalloys have been widely applied to

produce turbine blades for advanced gas turbine engines [1,2]. At pres-
ent, the Bridgman directional solidification (DS) is the major production
⁎ Corresponding author at: State Key Laboratory for Manufacturing System technique of SX blades. With the demands on the blade durability and
Engineering, School of Mechanical Engineering, Xi'an Jiaotong University, Xi'an 710049,
China.
reliability increasing, high crystal perfection of blade casting is being
E-mail address: fuwang@xjtu.edu.cn (F. Wang). pursued. During the DS process, many factors including alloy composi-
1
The two authors contributed equally to this work. tion, process parameters and blade geometries have impacts on the

https://doi.org/10.1016/j.matdes.2020.109138
0264-1275/© 2020 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
W. Xu, F. Wang, D. Ma et al.
grain growth. Hence the solidification process should be well controlled
to avoid grain defects which destroy the microstructural integrity by in-
troducing grain boundaries (GBs). Owing to the SX Ni-based superalloys
are lack of GB strengthening elements, the GBs usually become the
weakest positions under high temperature operating condition,
resulting in degradation of blade mechanical properties [3,4].
Over the past few decades, great efforts have been made to provide
insight to the grain defect formation [5–12], including stray grain (SG),
freckle, and low angle grain boundary (LAGB). However, limited study
on sliver can be found in literature. Sliver is generally characterized as
the misoriented grain extending along the solidification direction.
Their formation and evolution are not fully understood until now. In
the early study on the process window of single crystal castings [12],
slivers were considered as stray grains arise from the undesired nucle-
ation in the undercooling melt at the front of the solid/liquid interface,
due to poor process condition. It has been also reported that slivers usu-
ally originated at the inner surface defects of ceramic mold. The
misoriented grain formation could be attributed to the heterogeneous
nucleation facilitated by mold surface defects [13]. However, the nucle-
ated grains are normally of random orientation [14], whereas the major-
ity of sliver grains exhibit low deviation from the matrix. Thus, the
nucleation mechanism may be difficult to support the observation.
It has been suggested that dendrite deformation in the mushy zone
during the solidification process could cause sliver defects. Various fac-
tors including the instability of temperature field, the complex shape of
castings, the fluid flow during solidification, oxide inclusions, and ther-
mal stress have been correlated to the dendrite misorientation. Newell
et al. [7] found that dendrites exhibited random orientation deviation
under steady growth conditions and the maximum deviation was ap-
proximately 2.3°, while those under non-steady-state growth condi-
tions had the accumulated misorientation up to 6°. The increased
misorientation was attributed to the plastic deformation of dendrites
within the mushy zone. In addition, Siredey et al. [15] suggested that
the thermal stress caused by precipitation process of the γ' phase gave
rise to the dendrite deformation. The study by Xie et al. [16] on solidifi-
cation process of large-scale SX blades confirmed that the dendrite array
in the longitudinal direction gradually became disordered with the
height of casting increase during the DS process. And the occurrence
of dendrite misorientation tended to increase with the height.
Hallensleben et al. [17] provided an experimental evidence for dendrite
bending by measuring the dendrite growth deviation angles. Their re-
sults showed that the dendrite continuous bending angle could reach
1.7° over a distance of 25 mm. From above mentioned studies, it can
be summarized that the dendrite orientation would gradually vary dur-
ing successive growing.
Furthermore, Carney et al. [18] reported that slivers were frequently
observed where cross section of castings reduced. And the formation of
defect was attributed to oxide inclusions and the enhanced shrinkage
driven fluid flow. However, recent studies [19–21] showed that the
growing dendrites would be deformed at the enlarged cross section po-
sition due to local thermal stress concentration, and the deformed den-
drites further developed to misorientation grains. An in-depth study by
Aveson et al. [22] suggested that slivers arose as a result of the local
thermal stress at a sensitive position on the casting (the thin channel
upon seed) during seeded Bridgman DS process. They quantified the
dendrite misorientation using a tailored analysis method and evaluated
the stress field by numerical simulation. The experiment results indi-
cated that the differential thermal contraction between the mold and
the semi-solid alloy produced bending moments and torques on the
growing dendrites. The dendrites at the mold wall deflected and finally
developed to sliver grains. The defect formation was also correlated to
the geometric relationship between the dendrite growth direction and
the inner surface of mold wall.
According to the previous studies, sliver is characterized as a type of
grain defect formed by misoriented dendrite on the casting surface. The
defects observed at specific positions indicated its formation is
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Materials and Design 196 (2020) 109138
geometric sensitive. However, its formation mechanism remains less
well understood owing to the complexity of dendrite growth behavior
during solidification. It was observed that slivers would occur not only
in specific regions on castings, but also in the airfoil region without
structural discontinuity. Therefore, more efforts should be made to pro-
vide new insights into the defect formation mechanism. In this work,
sliver morphological features, misorientation range, and microstructure
of defect initiation points were examined. The effect of solidification
condition and airfoil geometries on the dendrite misorientation were
also analyzed. This investigation provided a direct experiment evidence
for dendrite deformation during directional solidification and a better
understanding of the sliver defect formation mechanism.
2. Experimental procedures
2.1. Experiment and characterization
Various SX castings were prepared by Bridgman directional solidifi-
cation (DS) combined with grain selection technique. Commercial
nickel-based superalloy CMSX-4 was used in the experiments. The DS
experiments were conducted with fixed process parameters in an in-
dustrial Bridgman furnace (ALD Vacuum Technologies, Inc.). The mold
preheating temperature and the alloy melt pouring temperature were
1500 °C. A withdrawal rate of 3 mm min−1 was used. After the DS pro-
cess, the castings were cleaned and macro-etched by an etchant (a
mixed solution of 50 vol% H2O2 and 50 vol% HCl) to reveal the grain
morphology. Then the castings with sliver defect were picked out for in-
vestigation. For microstructural observation, the regions containing
sliver defect were extracted by electro discharged machining. The sam-
ple surfaces with sliver defect were carefully polished and etched using
a solution containing 20 mL C2H5OH, 40 mL HCl, and 2 g CuSO4‧5H2O.
The dendritic structure was characterized by light microscopy (LM,
Zeiss Axio Vert.A 1 and Stemi 305). The microstructures of grain bound-
aries were observed by a scanning electron microscope (SEM, Zeiss
GeminiSEM 500). Energy Dispersive Spectroscopy (EDS) analysis was
performed to investigate the element distribution within the casting
samples. After the LM and SEM observation, the samples were polished
using an iron beam milling system (Leica EM RES102) For electron back-
scatter diffraction (EBSD) analysis. The crystal orientation was mea-
sured by using the HKL channel 5 package according to the EBSD data
collected by an EBSD detector (Oxford instruments). Furthermore, a
thin specimen across the GB between misoriented dendrite and matrix
was prepared by focus ion beam technique (FIB, Tescan Lyra3) and then
observed by a transmission electron microscope (TEM, FEI F200X Talos).
The FIB specimen was also examined by a EBSD system in TEM in order
to reveal the GB features.
2.2. Numerical simulation
The directional solidification process of blade casting was simulated
using a commercial finite element software (ProCAST, ESI Group), in
order to investigate the solidification condition for defect formation. Fi-
nite element model was built according to the actual dimensions of fur-
nace, ceramic shell, and blade casting. The mold temperature, alloy
melting temperature, and withdrawal rate used in simulation were con-
sistent with those applied in the experiment. A 1/6 model of the six-
blade cluster mold was used in consideration of the calculation effi-
ciency. The thermophysical parameters of CMSX-4 superalloy was ob-
tained from ProCAST calculation and Ref. [23], as shown in Table 1.
Some interpolation and extrapolation have been used to estimate the
data up to 1500 °C. Other simulation parameters were properly defined
based on literatures [24–26] and temperature measurement in our pre-
vious study [27]. In the stress simulation for alloy, isotropic elasto-
plastic model was employed. The mechanical properties of superalloy
in [001] orientation were used in the simulation, thus the anisotropy
[28,29] was ignored. The availability of this model to semi-
W. Xu, F. Wang, D. Ma et al.
Table 1
Material data of superalloy from ProCAST calculation and Ref. [23] (20−1500 °C).
Density (g/cm3) Thermal expansion (×10−6 K−1) Poison's ratio
7.5~8.5 6~19 0.36~0.5
quantitatively study the stress and strain characteristics of casting dur-
ing directional solidification has been checked by previous studies
[20,23,24]. In addition, the ceramic shell was set as a rigid body in
order to eliminate shell deformation, thus the stress in simulation
mainly reflects the thermal stress caused by shrinkage. For evaluation
of the stress in mushy zone, the stress calculation initiated at solid frac-
tion (fs) of 0.5.
3. Results and discussion
3.1. Defect morphology
3.1.1. Defect classification
Based on the grain defect inspection of many SX castings, it was
found that the slivers had various morphologies. They were linear sur-
face defects extending along the solidification direction. The width
ranged from a single dendrite to several dendrites, and the length
ranged from a few millimeters to tens of millimeters. For most of the de-
fects, the initial point can be clearly identified. The sliver defects can be
classified into three types according to the morphological features. The
first type was a subgrain formed by a segment of dendrite arm, the sec-
ond type was that containing an elongated misoriented dendrite, and
the third was a developed grain containing a cluster of misaligned den-
drites which derived from a misoriented dendrite, as shown in Fig. 1(a–
c). Generally, the development of sliver grains causes more serious
damage to the crystal imperfection of SX castings.
3.1.2. Defect initial point
An undeveloped sliver and its EBSD results are shown in Fig. 2. This
defect was observed near the trailing edge on a blade convex surface.
The dendrite growth direction converged to the mold wall and the den-
drite trunks showed a continuous growth morphology. The dendrite
array grew unidirectionally such that the misorientation defect was
hard to be found, as shown in Fig. 2(a). It was observed that a part of pri-
mary dendrite differed from the matrix in optical contrast. The EBSD
measurement confirmed this dendrite segment were about 1.5 mm in
length and had an abrupt change in crystallographic orientation, as
Fig. 1. (a) A sliver defect formed by a segment of dendrite (type 1) on blade convex surface. (b) Longitudinally developed sliver defects (type 2) near blade leading edge. (c) A
longitudinally and horizontally developed sliver defect (type 3) on blade concave surface.
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Materials and Design 196 (2020) 109138
Young's modulus (GPa) Yield stress (MPa) Ultimate stress (MPa)
0.5~127 0~960 0~1195
shown in Fig. 2(b–d). The inversed pole figures show that its orientation
in the longitudinal growth direction was almost the same as that of the
matrix, whereas the orientation varied in the other two directions, indi-
cating that this misoriented dendrite trunk rotated around the crystal
axis during solidification. The point to origin misorientation profile
along the dendrite growth direction shows that the sliver grain deviated
from the matrix at about 3.2° and kept a constant misorientation (Fig. 2
(d)).
It is interesting to note that the misorientation of dendrite trunks
within matrix was identified by EBSD measurement, as shown in
Fig. 2(b), and the typical low angle grain boundaries (LAGBs) were indi-
cated by white dash lines. A slightly misoriented dendrite adjacent to
the sliver was adopted for comparison of misorientation level. By
EBSD line scanning across the LAGBs, the misorientation values of the
two dendrite trunks were measured to be around 1°. These dendrites
may deflect during solidification and then fracture after the deformation
reaches a critical value. This result indicates that the sliver defect origi-
nated from a segment of misoriented dendrite trunk and the dendrite
segment detached from its parent arm owing to deformation.
3.1.3. Defect evolution
An elongated sliver (close to the leading edge of a dummy blade)
was adopted to explain the defect evolution, as shown in Fig. 3(a).
This sliver was observed at the side where dendrites converged to the
mold wall. It was found that the sliver originated from a misoriented
dendrite and developed to a narrow misoriented grain. Competitive
growth between the sliver and matrix dendrite trunks was observed.
The sliver dendrite was eliminated after it developed to a height of ap-
proximately 40 mm. The defect initial site can be readily observed, indi-
cating that the grain has an abrupt change in orientation (Fig. 3(b)).
Compared with the growing direction of matrix dendrites, this
misoriented dendrite deviated to the right side at approximately 8°.
Therefore, a diverging GB is formed at the left side, while a converging
GB formed at the right side, as shown in Fig. 3(c). During directional
growth, the secondary arms (S) of the misoriented primary dendrite
trunk (P) acquired sufficient space to branch ternary arms (T) at the di-
verging GB. The sliver grain grew upwards by deriving higher order
W. Xu, F. Wang, D. Ma et al. Materials and Design 196 (2020) 109138

Fig. 2. (a) Macrostructures of a sliver grain and a deflected dendrite. (b) EBSD orientation image map. Typical LAGBs along dendrite trunks are highlighted by the white dash lines.
(c) Corresponding inverse pole figure. (d) Point to origin misorientation line scanning along the white arrow in (b).

arms to form new longitudinal dendrite trunks (Fig. 3(c) and (d)) at this
side. However, at the converging GB, the secondary arms were blocked
by matrix dendrites. This observation was consistent with the widely
accepted model of competitive grain growth [30,31]. In fact, the den-
drites competitively grew in three-dimensions. In the observation
plane of this misoriented dendrite, the longitudinal growth was
terminated owing to branching was restricted and the dendrite tip
was geometrically constrained by the matrix dendrites and mold wall
(Fig. 3(e)).
The development of sliver defects can be correlated to the local
growing condition, including orientation [30], thermal field [31], and
growing space [20]. Thus, if the misoriented dendrite was under a

Fig. 3. (a) Overview of a typical longitudinally developed silver defect. (b) Defect initiation point. (c) and (d) Defect developing morphologies (in sequence). (e) Defect terminal.

4
W. Xu, F. Wang, D. Ma et al.
preferred condition for transverse and longitudinal propagation, it could
develop to a columnar grain with large size in both of cross section and
length. For instance, the developed sliver (type 3) shown in Fig. 1(c). It
is interesting to note that this sliver even grew through the platform and
into the blade root region.
3.1.4. Misorientation features
Morphology analysis and crystallographic orientation measure-
ments were carried out for a variety of sliver defects, in order to inves-
tigate the misorientation features. Misorientation of typical slivers is
shown in Fig. 4(a), the measurements were conducted within the defect
origin region. The deflected dendrite and the sliver defect shown in
Fig. 2 were also adopted for comparison (Fig. 4(b) and (c)). Two typical
slivers and corresponding inverse pole figures are shown in Fig. 4(d)–
(g), respectively. It was found that most of the slivers formed at the
side where dendrites converged to the mold wall. These slivers derived
from misoriented dendrite trunks and showed relatively small devia-
tion with respect to matrix. And the sliver orientations changed
abruptly rather than deviated with an accumulative misorientation
from the matrix. The abrupt-changed misorientation angles of sliver
grains ranged from 3.2° to 11.4°, whereas the typical accumulative mis-
orientation of dendrite bending was reported to be 0.68°/cm [17]. Addi-
tionally, the misorientation could be observed in all the three
crystallographic orientation ([001], [010], and [100]), indicating that
the sliver dendrites deviated from the matrix three-dimensionally
(Fig. 4(f) and (g)).
The experiment results support the defect formation mechanism
that a sliver originates from a segment of dendrite detached from the
matrix and indicate the angle of 3.2° may be the critical value for den-
drite fracture. Moreover, the small deviation partly explained why
slivers could co-grow with the matrix dendrites for a certain distance.
In comparison to freckle, which is also a type of surface defect arising
from dendrite fragmentation during directional solidification, slivers
generally occur individually and show successive growing morphol-
ogies similar to normal dendrites of matrix. Whereas freckles are char-
acterized as discontinuous and long chains composed by fine equiaxed
grains. Owing to the strong thermosolutal convection, the orientations
of freckle grains usually deviate from the matrix significantly and ran-
domly. Some freckle grains could develop to elongated grains similar
to slivers in morphology [10,32]. However, they usually form high
Fig. 4. (a) Misorientation distribution of typical slivers. (b)–(e) Defect morphologies of sample 1, 2, 4, 8, respectively. (f) and (g) Inverse pole figures for sample 4 and 8, respectively.
5
Materials and Design 196 (2020) 109138
angle grain boundaries and show less morphological correlation to the
ordered dendrites.
3.2. Microstructure analysis
3.2.1. Defect origin
The morphology and orientation measurements of a typical sliver
defect are shown in Fig. 5. This sliver was observed near the trailing
edge on a blade convex surface. It can be observed that the dendrite
growth direction converged to the mold wall and a segment of primary
dendrite trunk with a length of about 4 mm detached from the original
dendrite trunk. The location of the fracture can be clearly observed and
the dendrite array showed successive growth morphology, indicating
the dendrite detached without significant movement, as shown in
Fig. 5(a) and (b). The EBSD analysis results illustrated this segment of
dendrite maintained the original orientation in longitudinal direction,
but slightly deviated in the secondary orientation, in comparison to
the matrix (Fig. 5(c)).
The local magnified SEM image of sliver origin shows a layer of
coarse γ' precipitated along the GB and the coarse γ' were approxi-
mately 2 mm in length and 1 mm in width (Fig. 5(d)). The morphology
illustrates that the sliver originated from a fragmented dendrite and the
detached dendrite rejoined with the matrix during solidification. A TEM
sample was cut off at the fragmentation interface by FIB for microstruc-
ture analysis (Fig. 5(e)). It was observed that the γ' precipitates near GB
within the TEM sample showed coarse and irregular morphology,
which were different to those previous observed in Fig. 5(d), as
shown in Fig. 5(f). This could be attributed to the variation of GB mor-
phology within different section.
3.2.2. Validation of dendrite deformation
The TEM sample was analyzed by EBSD technique in order to deter-
mine the local misorientation near the GB at a microscopic scale. As
shown in Fig. 6 (a) and (b), the GB was not straight but exhibited a zig-
zag morphology. In the light of γ' precipitates morphology shown in
Fig. 5(f), it was found that the irregular γ' precipitates distributed at
each side of the GB and their edges were constrained by the GB. This re-
sult indicates that the precipitates occurred after the GB formed.
The local misorientation map and corresponding orientation distri-
bution range were illustrated in Fig. 6(c) and (d), respectively. It was ob-
served that each side of GB has no significant accumulative orientation,
W. Xu, F. Wang, D. Ma et al. Materials and Design 196 (2020) 109138

Fig. 5. (a) Macrostructure of a sliver defect. (b) Magnified image of defect origin. (c) EBSD orientation image map (inverse pole fig. X and Y). (d) SEM image of GB. (e) FIB extracting position
at the GB. (f) FIB prepared sample showing the microstructure of GB region.

but maintained the inherent orientation, indicating that the dendrite
misorientation can be characterized by brittlely fragment of dendrite
rather than dendrite deform with large plastic strain. The point to origin
misorientation line scanning result along the white arrow in Fig. 6
(b) reveals that the misorientation value jumped at the GB (Fig. 6(e)).
The orientation difference between the original grain and sliver was
measured to be about 5.7°. The pole figure of the investigated region
shows that the orientation deviation mainly occurred in the secondary
orientation of dendrite, as shown in Fig. 6(f), which was consistent
with the EBSD measurement results in dendrite scale (Fig. 5(c)).
The selected area electron diffraction (SAED) result of the GB region
in TEM sample suggests that the GB angle was about 5.7° and formed by

Fig. 6. (a) Band contrast image of the GB region within TEM sample. (b) Corresponding EBSD orientation image map. (c) Local misorientation map. (d) Local misorientation distribution.
(e) EBSD line scanning result along the white arrow showing in (b). (f) Corresponding pole figure.

6
W. Xu, F. Wang, D. Ma et al.
Fig. 7. (a) TEM image exhibiting the GB and (b) selected area electron diffraction (SAED) pattern of the GB region (white circle in (a)).
a grain rotating around the [001] zone axis (Fig. 7). This result confirms
that the segment of dendrite trunk rotated during solidification and
finally fragmented and developed to a sliver defect in turn.
A high-resolution TEM (HRTEM) image of the GB region and magni-
fied images of selected regions are shown in Fig. 8(a–f). Fast Fourier
Transform (FFT) was applied to the high-resolution image and then In-
verse Fast Fourier Transform (IFFT) was applied to the paired (200)
spots in the FFT spectrum in order to obtain the corresponding lattice
fringe image of the crystallography plane, as shown in Fig. 8(g–k). The
GB shows tilt characteristics, with periodic dislocation can be observed
at the GB, as shown in Fig. 8(b) and (g). These dislocations were the ge-
ometry necessary dislocations (GNDs) to form the GB. Furthermore, it
should be noted that various dislocations and lattice distortions can be
observed near the GB. These crystallographic defects were caused by a
certain amount of plastic deformation, which would be correlated to
solidification stress. The white dotted circle in the IFFT figure shows a
dislocation dipole (Fig. 8(i)). And dislocation loops were also observed,
as shown in white circle in Fig. 8(j). It is interesting to note that the ob-
served dislocation density was lower than that within the as-cast micro-
structure which would cause recrystallization [24]. The critical plastic
strain introduced in solidification process (above 1000 °C) for recrystal-
lization of CMSX-4 superalloy was estimated to be 1.5–2.0%, which is at
a relatively low level of deformation. Therefore, it suggests that the den-
drites were vulnerable during solidification and the required plastic
deformation would be quite small for the fragmentation.
Besides, a tertiary dendrite arm detached from its parent trunk was
observed, as shown in Fig. 9, further confirming that dendrites could
fragment mechanically and give rise to sliver defects. The dendrite frag-
mentation occurred at the junction between the primary and secondary
arm. And the tertiary arm exhibited a few misorientation level, indicat-
ing that it detached after branching and was mechanically constrained
by neighboring dendrites. This observation is consistent with the analy-
sis of deformation susceptibility of dendrite arms by Aveson [22] and
Takaki [33]. Niederberger [34] indicated that misorientation could be
more concentrated in dendrite branching necks due to the increased
local stress in such thinnest sections.
According to the above analysis, dendrites would mechanically
deform and fragment if the stress exceeds the mechanical strength
limit [35], resulting in the formation of sliver grains. In this study, it
was also found that oxide inclusions and pores could facilitate the sliver
formation. For instance, a longitudinal developed sliver defect accompa-
nied with oxide inclusions and pores was observed on the casting sur-
face (pointed out by a black arrow in Fig. 10(a)). The sliver grain had a
misorientation angle of 11.1° (Sample 7 in Fig. 4). The irregular pores
7
Materials and Design 196 (2020) 109138
were discovered after mechanical polishing (pointed out by yellow ar-
rows). Such pores were formed by insufficient liquid feeding into the
interdendritic region during the last stage of solidification and pro-
moted by solidification shrinkage [36]. The SEM morphology of a typical
pore is shown in Fig. 10(b). It was observed that the microstructure was
separated and partially rejoined. In the rejoined region, complex micro-
structure including coarse γ', oxide inclusions, and cracks was observed,
as shown in Fig. 10(c). EDS map shows the oxides contained alumina,
which may come from mold surface or oxide film during melting
(Fig. 10(d)). In the separation region near the pore, successive micro-
structural tearing was observed. The morphology of a crack with
rough interface shown in Fig. 10(c) indicates that the crack occurred
after solidification and was caused by thermal stress during cooling. Fur-
thermore, the surface within the pore shows the presence of many
spherical particles, which were considered to be the low melting point
phases formed at the last stage of solidification [37], suggesting that
the pore formed during solidification (Fig. 10(f)). This observation re-
sult demonstrates that dendrites would be subjected to complex stress
during solidification due to the presence of inclusions and pores, and the
dendrite fragmentation could be induced by the stress. Additionally,
whether the pore formation before or after dendrite deformation is
not clear according to the present experimental results. Both of the
two situation would cause higher susceptibility of dendrite fragmenta-
tion. Further investigation is required to improve the understanding of
the interaction between the pores and slivers.
So far, only the deviation of crystallographic orientation can be
found in previous studies on dendrite deformation, while the typical mi-
crostructure to reveal the mechanical deformation mechanism has been
rarely reported. The direct observation of dendrite deformation by X-
ray radiation imaging during the growing process [38] provided an ex-
perimental evidence for the dendrite deformation, however it did not
identify the inducing factors of defect formation and examine the mi-
crostructure features of the defect initiation point. The experimental re-
sults in this section support the sliver formation mechanism which
involves the dendrite mechanical deformation and fragmentation.
3.3. Critical solid fraction range
The small deviation range of slivers suggests that the dendrites
should be constrained by neighbor dendrites and have limited deflec-
tion space if they detached from the parent dendrites during solidifica-
tion. It would be reasonable to assume that the dendrite deflection
occurred at the last stage of solidification, at which the solid phase in
the mushy zone reached a relatively high content, and the dendrite
W. Xu, F. Wang, D. Ma et al.
Fig. 8. (a) High resolution TEM image of the GB region. (b–f) Magnified image of selected region in a. (g–k) Corresponding IFFT images of (b-f) constructed by using the (200) frequencies
in the FFT image.
network formation was almost complete. At this stage, the inter-
dendrite permeability sharply decreased [36], therefore the dendrite
deformation may not be caused by the liquid flow. However, the shrink-
age and deformation of the fully solidified part of the casting would be
transferred to the solid-liquid phase in the mushy zone [39]. Wang
et al. [40] indicated that when the solid fraction (fs) in the mushy zone
8
Materials and Design 196 (2020) 109138
reached 0.9~0.94, the dendrites were not bridged but surrounded by a
very thin liquid film. Hence the dendrites were vulnerable to the me-
chanical stress at this stage. At the bottom of mushy zone, the dendrites
coalesced with each other and acquired sufficient strength to withstand
the solidification stress. Whereas the dendrites at the top of mushy zone
were surrounded by liquid and had few mechanical constrains, such
W. Xu, F. Wang, D. Ma et al.
Fig. 9. The sliver defect formed by a misoriented tertiary dendrite arm (pointed out by a
red arrow). The defect originated from the thin neck of a secondary dendrite arm
indicating the dendrite deflection was associated with stress concentration.
that they were less affected by solidification deformation. Note that the
freckles are prone to form at the top of mushy zone due to high perme-
ability for liquid flow [32].
Our previous work [41] on the directional solidification characteris-
tics of CMSX-4 superalloy shows that the secondary dendrite arms par-
tially contacted when the solid fraction reached above 0.6. At a solid
fraction of 0.8, the secondary dendrite arms coarsened and overlapped
between the primary dendrite arms, resulting in a morphology similar
to that of the solidification completion. Fig. 11(a) is a schematic diagram
of dendrites in the mushy zone showing solid volume fraction change
during directional solidification. The transverse sections of mushy
zone at solid fraction of 0.4, 0.6, and 0.8 are shown in Fig. 11(b), (c),
and (d), respectively. The dendrite morphologies of different solid frac-
tions combined with the low deviation level of sliver grains (mentioned
in 3.1.4 section) suggest that dendrite fragmentation causing slivers
Fig. 10. (a) Macrostructure of the sliver defect. (b) SEM image of a typical pore. (c) Magnified image of the rejoined region in (b). (d) EDS mapping analysis result on O and Al distribution
for the region shown in (c). (e) Crack interface showing microstructural tearing. (f) The inner surface of a pore.
9
Materials and Design 196 (2020) 109138
occurred when the solid fraction reached 0.6 to 0.8 during directional
solidification.
3.4. Solidification deformation analysis
According to the above analysis, the dendrites in the mushy zone
would be affected by solidification deformation. Moreover, the observed
dendrite misorientation showed a strong tendency at the converging
side where the dendrites grew to the mold inner wall. This result is con-
sistent with the observations of Aveson et al. [22]. It may be attributed to
an extra load or constraint on dendrite arm due to the interaction with
the mold wall. Bogdanowicz et al. [42] reported that the mechanical in-
teraction between growing dendrites and mold wall could induce a
forced orientation effect on dendrites at the converging side of thin-
walled blade, resulting in the misorientation defect.
In order to investigate the influence of solidification deformation, the
solidification process was analyzed by ProCAST simulation. The simulated
thermal profile of airfoil region during solidification process is shown in
Fig. 12(a). It was found that a concave solidification front formed. And
the solidification front inclined to the heater side due to the convex surface
of airfoil faced to the heater. The curved solidification front could influence
the dendrite growth in two aspects [17,43]. First, primary dendrites tend to
grow perpendicular to the liquid isotherm. Hence dendrites within high
curvature region may be prone to deform. Second, a concave solidification
front would assist secondary dendrite arms to preferentially branch to-
ward the casting center. This may result in overgrowth of sliver grains
from outer region to the casting central region. In the present study, no suf-
ficient evidence was found to indicate that the high curvature inevitably
leads to sliver formation or offers slivers more favorable growth conditions.
In consequence, there is a need to further identify the influence of thermal
field on sliver formation and evolution.
The stress contours within an airfoil cross section at a solid fraction
of around 0.7 is shown in Fig. 12(b). Owing to the unstable thermal
W. Xu, F. Wang, D. Ma et al. Materials and Design 196 (2020) 109138

Fig. 11. (a) Schematic of dendrites in the mushy zone showing solid volume fraction (fs) change during directional solidification. (b–d) Transverse sections of mushy zone at solid fraction
of 0.4, 0.6, and 0.8, respectively [41].

Fig. 12. (a) thermal profile of airfoil during solidification process. (b) Effective stress contour in mushy zone at solid fraction of ~0.7. (c–e) Corresponding displacement of X, Y, and Z,
respectively. (f) Schematic illustration of the component forces applied on the dendrite near casting surface.

10
W. Xu, F. Wang, D. Ma et al.
Fig. 13. (a) Schematic of typical blade cross-sections, (b) schematic of blade cross sections (S1 and S2), and (c) longitudinal section (S3).
field, the effective stress within mushy zone distributed non-uniformly.
The corresponding displacement in X, Y, and Z axis are shown in Fig. 12
(c), (d), and (e), respectively. It can be observed that the casting had
non-uniform deformation in both transverse and longitudinal direc-
tions during solidification. The airfoil tended to shrink inward and
downward. Thus, the complex shrinkage should have impact on the
dendrites in mushy zone. Therefore, the vulnerable dendrites are
prone to deflect if suffer from an unbalanced stress field. For an individ-
ual dendrite on the casting surface, the complex interaction with sur-
rounding dendrites and mold wall involves in the deformation
process. The stress acted on the dendrite could be considered as the re-
sultant of multiple stresses in different directions and equivalents to a
stress parallel to Z axis (σZ, tensile or compression) and a stress in X-Y
plane (σXY, shear), as shown in Fig. 12(f). The inward and downward so-
lidification shrinkage contributes to the resultant stress. For instance,
downward shrinkage leads to the tensile stress on dendrite arm, while
the torque in X-Y plane which could arise from inward shrinkage as
well as the interaction between dendrite and mold wall results in the
rotation of dendrite trunk.
Another factors to take into consideration for the dendrite deflection
is the width of mushy zone. The width of mushy zone is inversely pro-
portional to the longitudinal thermal gradient within mushy zone. Dur-
ing the solidification process of SX blade by conventional DS method,
the thermal gradient would gradually decrease with the increase of
casting height, hence the mushy zone will become wider [26,44]. More-
over, the solidification front on shadow side usually possesses a wider
mushy zone [45,46]. With lower longitudinal thermal gradient within
mushy zone, the stay period of dendrites in the vulnerable zone
would be prolonged. Hence the risk of dendrite deflection further
increases.
3.5. Effect of airfoil geometry
The airfoil of turbine blade possesses complex three-dimensional
curved surfaces, i.e. convex surface and concave surface. In the direction
along the blade vertical axis, the cross section from the airfoil tip to the
bottom is characterized by a continuous twist. Within the airfoil region
of the blade casting shown in Fig. 1, the typical cross-sections (S1 and
S2) stacked along the blade vertical axis (Z) from the tip to bottom
(Fig. 13(a)). It can be seen that the twist made the leading edge contour
moved to the side of convex surface, while the position of trailing edge
changed insignificantly (Fig. 13(b)).
In the directional solidification process of SX blade, the selected
grain is usually introduced from the blade tip and the withdrawal direc-
tion is parallel to the blade vertical axis. Therefore, it is inevitable that
11
Materials and Design 196 (2020) 109138
the growing dendrites contact with the mold wall due to the airfoil ge-
ometry. As shown in a typical longitudinal cross-section (S3) parallel to
the vertical axis, the airfoil surface had an inclination (Fig. 13(c)). If the
primary dendrites grow parallel to the vertical axis, a converging inter-
face will form on the convex surface, while a diverging interface will
form on the concave surface. The converging and diverging angle
were denoted by α and β (Fig. 13(c)), respectively. This model predicts
that the sliver has a higher probability to occur on the convex surface,
owing to the dendrite deformation susceptibility at converging inter-
face. The occurrence of sliver defects near the leading edge on the con-
vex surface, as shown in Fig. 1(a), was consistent with the prediction. In
this region, the local dendrite growth direction slightly converged to the
mold wall (almost parallel to the surface), according to the observation
of dendrite growth orientation within casting. In addition, other factors
including the grain orientation, solid-liquid interface morphology, and
the size of dendrite arms [20,47,48] would also affect the dendrite de-
flection as well as sliver formation. Thus, the sliver defect could occur
at the concave surface, as shown in Fig. 1(c), when the selected grain
orientation largely deviates to this surface (the interface becomes
converging).
Statistics on sliver defects in the SX blade casting production showed
that various slivers occurred more frequently on the convex surface,
whereas a few defects were detected on the concave surface [49]. To
some extent, the influence of airfoil structure discussed in this section
can be used to explain the defect formation susceptibility in the indus-
trial production. Besides, several studies [14,50,51] reported that slivers
could occur at the diverging interface. Their formation mechanisms may
be slight different, but they are still associated with dendrite deforma-
tion. For fully understand the dendrite deformation mechanism, further
investigation is required.
3.6. Defect prevention
Previous studies have reported that low angle grain boundaries de-
teriorate mechanical properties, particularly the GB angle exceeds 9°
[52]. The GB misorientation tolerance of several alloys is even lower
than 6° [53]. According to the experimental results, the misorientation
of sliver defects could exceed 9°. Some fragmented dendrites would de-
velop to narrow misoriented grains or large three-dimensional colum-
nar grains to damage the SX structure. Generally, misorientation
tolerance and defect occurrence position are established to allow the
presence of slivers in order to reduce the production cost of SX blades.
However, for new generation engines demanding higher durability, it
is necessary to minimize the occurrence of the sliver defects within SX
turbine blades. The formation and evolution mechanism of such defect
W. Xu, F. Wang, D. Ma et al.
is complex, which involves solidification stress, temperature field, ge-
ometry, crystal orientation, etc. Eliminating the defects is still challeng-
ing. Several process optimization techniques can be taken into account
to reduce the rejection of castings. Except for grain orientation control
technique [22], optimization of process parameters [26] as well as the
casting arrangement in cluster mold [54] are needed in order to reduce
the width of mushy zone and the inclination of solid–liquid interface.
Several modification of DS equipment, such as square heater [3] and ra-
diation baffle [46] can be considered to reduce the curvature of solidifi-
cation front. Moreover, the mold quality must be strictly controlled,
especially the inner surface of the mold should be smooth and clean,
in order to prevent the localized stress during solidification. Also, reduc-
tion of oxide inclusions in melting and pouring process is necessary.
4. Conclusions
In the present work, we investigated the formation of sliver defects
in single crystal Ni-based superalloy castings by analyzing the macro/
micro morphologies of defects and the solidification conditions. The
main conclusions can be summarized as follows:
(1) During directional solidification of SX castings, dendrite frag-
mentation arose the formation of sliver defect. The misorienta-
tion of sliver grain ranged from 3.2° to 12°. The minimum
misorientation of 3.2° may be the critical value for dendrite frag-
mentation. The EBSD orientation measurement and TEM obser-
vation of dendrite with slight deviation indicated that the
dendrites fragmented brittlely rather than with large plastic de-
formation.
(2) The dendrite fragmentation can be attributed to macroscopic and
microscopic non-uniform stress. And the dendrite deformation
included torsion and bending. Moreover, the oxide inclusions
and pores could induce dendrite fragmentation.
(3) The low misorientation level of sliver grain indicated that the
dendrite fragmentation occurred when the solid fraction of
mushy zone reached a high level. According to the dendrite mor-
phologies of different solid fractions in mushy zone, the possible
solid fraction range for fragmentation was suggested to be
0.6–0.8.
(4) The observation in this experiment showed slivers frequently oc-
curred at the side where the primary dendrites converged to the
mold inner wall. The sliver defects on the blade convex surface
may be correlated to the formation of converging interface.
Credit author statement
Wenliang Xu: Data curation, Formal analysis, Investigation, Writing -
original draft. Fu Wang: Methodology, Funding acquisition, Writing -
original draft. Dexin Ma: Conceptualization, Validation, Writing - review
& editing. Xintao Zhu: Data curation, Investigation. Dichen Li: Supervi-
sion, Project administration. Andreas Bührig–Polaczek: Project
administration.
Declaration of Competing Interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influ-
ence the work reported in this paper.
Acknowledgements
This work was supported by the National Natural Science Founda-
tion of China (No. 91860103) and the Key Program of Equipment Pre-
Research Field Foundation of China (No. 61409230405). The authors
12
Materials and Design 196 (2020) 109138
acknowledge the support of the Youth Innovation Team of Shaanxi
Universities.
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