Solidification defects in directionally solidified

nickel base superalloys: problem solving

using electron backscattered diffraction
B. A. Shollock*
The production of high quality turbine blades from nickel base superalloys poses a challenging
problem for the aeroengine and power generation industries. The occurrence of defects in the
final single crystal component has become more common with the increasing complexity of the
components in the aerospace sector and the increasing size of the blades in industrial gas
turbines. In parallel, alloy development has improved the operating capabilities of these parts, but
these new generation alloys have encountered more casting difficulties. The defects that occur
are normally identified by metallographic and X-ray diffraction techniques. These approaches are
limited by the subjectivity of determining subtle changes in contrast and by the averaging over the
relatively large sampling volumes of the X-ray beam. Electron backscattered diffraction (EBSD)
provides a direct approach for identifying the nature of the defects formed in these castings. This
paper will present an EBSD driven assessment of problems encountered in directional
solidification of nickel base superalloys: the formation of stray grains in seeded single crystals
and the effect of alloy composition on the evolution of orientation. The origins of these defects will
be considered with respect to classical grain growth theory.
Keywords: Single crystal nickel base superalloys, Solidification, Electron backscattered diffraction, Directional solidification, Solidification defects

Introduction depends greatly on casting size. The solidification rate R

Single crystal superalloy processing provided one of the
key advances in the application of these alloys in high
efficiency aero- and land based gas turbines. Alloy
development, aimed mainly at increasing the c9 volume
fraction and solvus temperature, accompanied these
process advances. Investment casting of superalloys
through directional solidification to single crystal
production resulted in increased temperature capability
and thermal fatigue resistance. Growth of single crystal
superalloys is conducted in conditions of dendritic
solidification. Controlled uniaxial heat flow enables
dendrites to grow parallel to the axis of the casting
and natural grain selection is expected to produce a near
n001m axial orientation. McLean1 reported that the
solidification conditions necessary for columnar dendri-
tic growth must exceed a critical value of the ratio (G/
R)crit, where G is the temperature gradient at the solid/
liquid interface and R is the solidification rate. G and R
also govern the scale of the dendrites; the primary
dendrite arm spacing is given by lp!G21/2R21/4. The
heat transfer characteristics of the system determine the
value of the thermal gradient G, which as a consequence
Department of Materials, Imperial College London, London, SW7 2AZ, UK
*Corresponding author, email b.shollock@imperial.ac.uk
must satisfy the (G/R)crit condition.
Development of complex turbine blades requires both
engineering design advances and alloy development.
Design engineers now specify blades with specific off
axis n001m orientations and alloy compositions have
become more complex. Each of these factors compli-
cates the casting procedure, making high yield produc-
tion of quality castings very difficult. Although
straightforward axial growth of single crystal turbine
blades has become a matter of routine in the aeroengine
sector, for more complex components such as clusters of
nozzle guide vanes and shrouds, for aeroengines such as
the Trent 900 and for larger turbine blades used in
industrial gas turbines for electricity generation, control
of orientation and defects is proving difficult and further
complicated by the introduction of advanced alloys.
de Bussac and Gandin developed a strategy for the
prediction of successful investment casting of single
crystals, citing stray grains as a particular problem as
alloys used for single crystal turbine blades typically lack
additions of grain boundary strengthening elements.2
This paper illustrates the application of electron back-
scattered diffraction (EBSD) to aid the understanding of
the origin and development of solidification defects in
nickel base superalloys. Two types of defects encoun-
tered during investment casting of single crystal super-
alloys will be presented to illustrate the effectiveness of
EBSD in elucidating the defects and their origins.

ß 2006 Institute of Materials, Minerals and Mining

Published by Maney on behalf of the Institute
Received 13 December 2005; accepted 20 April 2006
1338 DOI 10.1179/174328406X130939 Materials Science and Technology 2006 VOL 22 NO 11
 Shollock
a b
1 a EBSD map of longitudinal section from CMSX-4 sam-
ple and b optical micrograph of longitudinal section:
grain boundaries have been outlined for clarity; note
lower magnification in b
Experimental
Examination of defects in castings of superalloys typically
involves complex etching procedures and a subjective
visual assessment of contrast and morphology to
determine the nature of the defect. Metallographic and
backscattered electron imaging in the scanning electron
microscopy (SEM) can also be used; however, because
optical and electron microscopy techniques are affected
by compositional differences inherent in the dendritic
structures, the only technique able to reveal changes in
orientation and all defects and stray grains within the
microstructure is EBSD. EBSD was carried out on
electropolished samples using two systems, a JEOL 840
SEM equipped with the HKL Channel 4.2 and 5.1
analysis packages, and a LEO Gemini field emission gun
SEM equipped with Oxford Instruments crystal analysis
and Channel 4.2 and 5.1 analysis packages.
Results and discussion
Stray grain nucleation
Industrial casting of turbine blades sometimes involves
the use of a non-n001m oriented single crystal seed to
2 Effect of casting distance on morphology and number of defect stray grains: grain length refers to length of largest grain
around the sample circumference while grain width refers to largest distance defect grains grow from edge toward centre;
only grains surrounded by high angle boundaries (.15u) have been included in the analysis; examples of transverse sec-
tions of 12 mm diameter casting analysed by EBSD used to determine these measurements are also shown
Solidification defects in directionally solidified nickel base superalloys
nucleate the desired orientation. The prefabricated seed
is placed in the mould, the entire assembly preheated
and then molten alloy is poured into the mould cavity.
During the preheating step, the top portion of the seed is
melted, producing a liquid/solid region in the seed,
referred to as the melt back mush. During casting, this
melt back region can be the origin of stray grains that
can result in defects in the final casting. Understanding
the origin of these melt back defects would help develop-
ment of an efficient transfer mechanism of orientation
from the high quality prefabricated seed directly into the
cast part. The grains originating in the melt back mush
are often invisible during conventional metallographic
analysis and EBSD has shown to be a valuable tool in
identifying them.3
Figure 1 indicates that the stray grains near the melt
back mush (within 5 mm) are confined to very near the
surface of the casting. Longitudinal sectioning perpen-
dicular to the cast surface was used to examine how this
depth changed with distance. An EBSD orientation map
of a CMSX-4 casting (Fig. 1a) shows that the stray
grains tend to be retained close to the casting surface
and persist a large distance in the casting direction. It
can be seen that EBSD reveals more information than
the metallographic section presented in Fig. 1b.
Defect grains were found to occur on the side where
the primary dendrites of the seed diverge from being
parallel to the mould wall. However, sectioning close to
the melt back shows little bias in stray grain nucleation;
rather, the nucleated grains are distributed uniformly
around the perimeter of the casting. The development of
these grains can be seen in Fig. 2.
Specifically, the side of the seed where the primary
dendrites of the seed diverge from being parallel to the
mould wall is where these grains develop; where the
dendrites converge on the mould wall the stray grains
are overgrown by the seed crystal. In non-n001m seeds,
on the side where the seed dendrites converge onto the
mould wall, defect stray grains are quickly outgrown
by the seed dendrites. Where the seed primaries and
the mould diverge, the stray grains are able to grow
secondary and tertiary arms to fill the space where the
seed dendrites grow away from the mould wall.
Materials Science and Technology 2006 VOL 22 NO 11 1339
Shollock Solidification defects in directionally solidified nickel base superalloys
3 Comparison of n001m pole figures of directionally soli-
dified CMSX-4 and CM186: sections are taken 22 mm
above chill
Effect of alloy composition
The composition of superalloys has evolved over five
generations, with the addition of refractory and transi-
tion metals becoming increasingly common in single
crystal alloys. As single crystal components are more
frequently demanded for high specification applications,
the complex geometries prove challenging for the
production of high yields. The influence of alloy
composition further adds to the situation. For example,
Tin and Pollock4 and Tin et al.5 report that the
thermosolutal convection that results in defects such as
freckles depends on both primary dendrite spacing lp
and alloy composition; below a certain value of lp, this
convection does not occur, and tungsten and rhenium
promoted freckle formation while tantalum and carbon
additions suppressed the formation of these defects.
EBSD can be used to demonstrate clearly the dif-
ferences in solidification behaviour of the alloys. The
compositions of two second generation superalloys,
CMSX-4 and CM186LC with similar compositions,
4 Orientation maps and n001m pole figures for diverging (left) and converging (right) boundary in bicrystals of CMSX-4: ver-
tical dotted line in orientation schematic diagrams represent the casting axis, while tilted one shows grain boundary
1340 Materials Science and Technology 2006 VOL 22
are 5.6Al–1.0Ti–6.5Cr–9.0Co–61.7Ni–0.6Mo–6.5Ta–6.0W–
3.0Re–0.1Hf and 5.7Al–0.7Ti–6.0Cr–9.0Co–62.6Ni–0.5Mo–
3.0Ta–8.0W–3.0Re–1.4Hf–0.07C (wt-%) respectively.6,7
These two alloys were directionally solidified in a
Bridgman furnace as cylindrical ingots with a with-
drawal rate of 180 mm h21 under a temperature
gradient of 5 K mm21, further details of the experi-
mental configuration can be found elsewhere.8,9 Figure 3
presents n001m pole figures presenting the final textures
resulting from directional solidification. The CMSX-4
casting shows more pronounced scatter in the preferred
crystallographic n001m orientations in comparison with
CM186LC.
Dsouza et al. demonstrated that the efficiency of
development of a sharp solidification texture is sensitive
to the principal solidification parameters, the magnitude
of the temperature gradient G in the liquid and the
growth rate V.10 In the present case, the solidification
texture that develops in the casting also depends on the
alloy composition.
EBSD has been shown to reveal important morpho-
logical and crystallographic information on the defects
formed during melt back and on the effects of alloy
composition on the final orientation. In order to
understand the mechanisms related to overgrowth in
superalloys, solidification of bicrystals was undertaken.
Bicrystals representing converging and diverging den-
drites were studied. The growth of these crystals was
conducted according to experimental procedures
detailed elsewhere.9 Metallographic and EBSD analyses
were conducted to elucidate the interactions between the
dendrites. In the EBSD maps presented in Fig. 4, the
large arrows at the bottom left indicate the orientations
of the primary dendrite trunks of the adjoining grains
relative to the ingot axis, which is given by the dashed
line. The deviation of the n001m crystallographic
NO 11
 Shollock
a b
5 Secondary dendrite arm formation in CMSX-4 in case
of a diverging grain boundary and b converging grain
boundary
direction of the growing grains from the ingot axis is
given above the relevant arrow and the number above
the dashed line gives the inclination of the grain
boundary to the ingot axis. Little lateral growth is
observed and the initial angle of inclination is preserved
as the grain boundary plane.
In the case of the converging grains, the grain
misaligned by 20u overgrows the more favourably
oriented grain. In contrast, for the diverging grains,
the less favourably oriented grain is overgrown by the
near n001m grain. In both cases, the grain boundary is
parallel to the more favourably oriented grain.
Figure 5 clearly shows the formation of secondary
dendrites in both the diverging and converging cases.
In the classical theory for competitive grain growth by
Walton and Chalmers, the grain selection mechanism is
based on the principle that the n001m crystallographic
direction is the fastest growing in the cubic system.11
They rationalised that the {001} planes are the least
densely packed and as the advancement of the solidifica-
tion front can be viewed as the attachment of liquid
atoms on the solid, these atoms are the most easily
accommodated in the least densely packed planes. A
dendrite growing at an angle to the direction of heat flow
must grow faster to have a component of velocity in the
solidification direction to equal the velocity of a dendrite
that is growing parallel to the direction of heat flow. The
dendrite oriented with the fast growing n001m orienta-
tion parallel to the solidification front will lead the
misoriented dendrite which requires a greater under-
cooling to maintain the same component of axial
velocity. The latent heat and rejected solute of the
leading dendrite retards the growth of its slower
neighbour. It is the thermal and solutal fields associated
with the secondary arms of the leading dendrite that
blocks the growth of the slower growing dendrite. In the
presence of a planar solidification front, Gandin and
Rappaz12 studied the competitive grain growth process
during directional solidification of an Inconel alloy and
showed a progressive clustering of grain orientations in
the centre of the {001} pole figure. Their findings are
consistent with the grain selection mechanism proposed
by Walton and Chalmers.
In the case of the converging grains, the grain
misaligned by 20u overgrows the more favourably
oriented grain, an inconsistency with the classical
theory of Walton and Chalmers.9 By combining the
Solidification defects in directionally solidified nickel base superalloys
observations from EBSD measurements and metallo-
graphic examination of the dendrite morphologies as
given in Fig. 5, a modified grain selection process can be
proposed. In the case of the converging grains detailed
in this paper, the impingement of the primary trunks
dominates the overgrowth process and solute rejection
by both dendrite tips inhibits the growth of secondary
arms producing a boundary parallel to the leading
dendrite with both grains experiencing suppression of
secondary arms. In the case of the diverging grains, both
grains continue to grow without competition with
secondary and tertiary dendrites filling the evolving
gaps between the grains. These observations in the
bicrystal are consistent with the observations of the
emergence of stray grain at the mushy zone in off axis
seeded crystals. Where the seed primary dendrites and
the mould wall diverge, stray grains are stable as they
are able to grow secondary and tertiary arms to fill the
space to the mould wall.
The classical model of competitive growth between
neighbouring dendrites proposed by Walton and
Chalmers has been shown to be inappropriate to account
for grain competition in chemically complex alloys such
as CMSX-4. The extent of microsegregation is probably
the most significant factor in the differences between
CMSX-4 and CM186 during directional solidification.
Detailed studies of the partitioning of elements in these
alloys have shown that in CM186 there is a greater
rejection of tantalum to the melt with the hafnium on this
alloy also partitioning to the melt. In addition, the
partitioning of rhenium to the dendrites is greater in
CM186 than in CMXS-4. It is likely that the diffusion of
rhenium, hafnium and tantalum in the melt of CM186 is
slow, reducing the solute interaction distances and
inhibiting the growth of secondary dendrites by reducing
the size of the solute diffusion field.4,11
Conclusions
EBSD has been shown to be a powerful tool at identifying
defects in directionally solidified nickel base superalloys.
The use of controlled bicrystal solidification experiments
of diverging and converging grains and subsequent EBSD
analysis has provided a vital insight into the mechanisms
of defect formation and its relationship to the existing
theory of competitive grain growth.
Acknowledgements
The author is grateful to Dr M. Ardakani, Dr
N. Dsouza, Dr P. Jennings, Dr N. Stanford and Dr
A. Wagner and Professor M. McLean. The support of
EPSRC, Rolls-Royce and Alstom are acknowledged.
References
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ture service’; 1983, London, The Metals Society.
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35–42.
3. N. Stanford, A. Djakovic, B. A. Shollock, M. McLean, N. Dsouza
and P. A. Jennings: Scripta Mater., 2004, 50, (10), 159–163.
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1342 Materials Science and Technology 2006 VOL 22 NO 11