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Oxide Defects in a Vacuum Investment–Cast Ni-Based

Turbine Blade
A.K.M.B. RASHID and J. CAMPBELL

Samples from large turbine blades for power generation, investment-cast in vacuum from a nickel-
based superalloy, were investigated. Samples were cut from regions near the top of the casting that
contained freckle defects. The microstructures of these segregated regions were compared with those
from nonsegregated adjacent regions using both optical microscopy and scanning electron microscopy
(SEM). The segregated areas revealed a high density of carbides and a network of cracks. Samples
were prepared by carefully fracturing along the cracks so as to observe the surfaces of the cracks.
Observation by SEM revealed the presence of inclusions identified as films that appeared to have
initiated the growth of carbides. Fractures of random areas of the nonsegregated alloy revealed that
the films were numerous and widely distributed. In all cases, the films were principally oxides (and/or
possibly nitrides) of aluminum and chromium. It was hypothesized that the films had originated by
entrainment of the surface film on the liquid metal during the turbulent pouring of the casting. The
films could, therefore, be assumed to be double, because the entrainment mechanism is a folding
action. It follows that the doubled-over films constitute (1) the observed cracks and (2) the substrates
for carbide precipitation. Evidence from other alloy systems is presented to support this conclusion.

I. INTRODUCTION tion will confirm that the entrainment of single-oxide films

NICKEL-BASED superalloys are generally used for the
production of high-performance turbines for power genera-
tion. The requirements for near-net shape, accuracy and sur-
face finish dictate that the blades are cast in investment molds
in a vacuum furnace.
However, because of the necessity for the investment wax
assembly to be robust, many investment castings use top-poured
gating systems. This undesirable filling technique introduces
the danger of the random entrainment of the surface of the liq-
uid metal into the bulk of the casting (Figure 1). Despite the
use of the vacuum for melting and casting, there is, of course,
plenty of residual air in the vacuum environment to ensure
that a surface film of oxide or nitride will form. This is espe-
cially true during the act of pouring, when the vigorous out-
gassing of the mold causes the “vacuum” (i.e., the dilute air
environment) to be momentarily severely contaminated. The
transient out-rushing of air as the mold is thermally shocked
is usually clearly signaled on the vacuum gages of the furnace.
During the turbulence of the pour, it is to be expected,
therefore, that oxides and, possibly, nitride surface films (the
aluminum and chromium in the alloy effectively gettering
the residual gases in the vacuum chamber) will be formed
on the falling liquid and, therefore, randomly folded into the
melt, dry side to dry side. These unbonded interfaces, separat-
ing thin but stable oxide layers, will act as cracks in the
liquid. Because of the mechanism of entrainment is a folding
mechanism, the films are necessarily always double and,
necessarily therefore, always act as cracks. A moment’s reflec-
A.K.M.B. RASHID, Professor and Head, is with the Department of Mater-
ials and Metallurgical Engineering, Bangladesh University of Engineering
and Technology, Dhaka-1000, Bangladesh. J. CAMPBELL, Professor of
Casting Technology, is with the Department of Metallurgy and Materials,
University of Birmingham, B15 2TT United Kingdom. Contact e-mail:
j.campbell.met@bham.ac.uk
Manuscript submitted March 4, 2003.
cannot occur.[1] Such doubled-over oxides, known as bifilms,
will be expected to be frozen into the casting and will act
as cracks in the finished component, threatening fatigue and
creep resistance.[1] There is evidence that random defects
introduced in this way are the cause of increased scatter of
mechanical properties.[2] In addition, in contrast to the struc-
tures observed in turbine-blade materials that have been cast
without significant turbulence, grain-boundary facets have
been observed on fracture surfaces of vacuum-cast Ni-based
alloys that had been turbulently poured.[3] Such planar fea-
tures are typical results of the flattening of tangled or crum-
pled bifilms by the progressive advance of a dendrite array.[1]
In this study, a number of investment-cast Ni-based super-
alloy turbine blades were investigated in detail. Particular
interest was targeted to demonstrate the presence of bifilms,
if any. Such features, although now known to be common
in metals cast in air,[1] are also predicted to be present in
vacuum-cast material, but have not previously been observed.
Their relative distribution in the bulk of the casting and in
the centers of channel defects (freckles) was also studied,
since it was thought that bifilms might be concentrated in
regions of the casting that are the last to solidify as a result
of being pushed ahead of advancing dendrites.[1]
II. EXPERIMENTAL PROCEDURE
The blades were investment-cast using a top-pour gating
system that consists essentially of a large funnel to guide
the falling melt into the top of the mold. The blade is oriented
with its heavy end upward. No filters were employed. Such a
simple system is conventional for such products, since,
despite efforts over many years, it has not been found possi-
ble so far to provide a bottom-gated filling system for large
turbine-blade castings that can survive the investment
shell–building process. The castings were cast from a TLV
8933–grade nickel-based superalloy, the principal alloying

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elements of which are shown in Table I. Normal casting
conditions included the mold preheat of 1000 °C and the
liquid-metal pour temperature of 1380 °C.
Samples were excised from turbine blades (Figure 2) pro-
duced in a commercial casting operation. Areas containing
the segregated regions constituting the channel (freckle) defects
were cut from the castings for metallographic observation
(Figure 3). The samples were cut and polished using standard
procedures to a finish of 1 m using diamond paste and then
etched in a saturated solution of cupric chloride containing 3:1
HCl:HNO3. Both unetched and etched samples were then obser-
ved using optical microscopy, a PHILIPS* XL30 scanning
*PHILIPS is a trademark of Philips Electronic Instruments, Mahwah, NJ.

electron microscope, and a PHILIPS XL30 environmental

Fig. 1—A schematic representation of a surface turbulence leading to the
entrainment of a double oxide film decorated with gas (air) bubbles.
Table I. Nominal Composition of the Nickel-Based Superalloy
scanning electron microscope–field-emission gun. Energy dis-
persive X-ray (EDX) was used to characterize chemically the
segregated and nonsegregated areas.
Finally, selected samples were carefully fractured along the
cracks observed to be present in the segregated areas. The
opened cracks were observed by scanning electron microscopy
(SEM). This is a powerful technique to reveal the presence
of bifilms, separated into its two halves analogous to the open-
ing of a butterfly’s wings. (From work on other alloy systems,
it was expected that the two films that constitute the bifilm
would be too thin to be easily detectable on a polished cross
section.) The matrix alloy well away from the segregated area
of the freckle defect was also fractured through a randomly
chosen region to reveal the typical alloy structure and com-
pare its defect content with that of the freckle region.

Al C Co Cr Fe Mo N Ti W Zr Total
III. RESULTS
3.00 0.16 9.32 14.08 0.17 4.02 0.002 5.05 3.88 0.019 100
When polished and etched transverse cross sections of
freckles were viewed under the optical and scanning electron
microscopes, they were found to contain a network of cracks
(Figures 4(a) and (b)). The freckle itself was approximately
5 mm in diameter. The maximum length of cracks contained
in the freckle was approximately 2 mm. The microstructure
inside the freckle appeared quite different from that of the
defect-free area of the casting. The normal matrix structure
(Figures 5 and 6) had little contrast, since there were few grain
boundaries and the carbon content was so low that there were
few MC carbides. In the segregated area, however, the accu-
mulation of eutectic carbides was clear (Figures 5(b) and 6(b)).
Figure 7 shows the fractographs of the freckle area opened
along one of the cracks. Areas of the fracture surface appear
to be films overlying a brittle phase.
The films were characterized by a light appearance in the
secondary electron image, possibly indicating a nonelectrically-
conducting phase that charged slightly in the electron beam.
On close examination, it appeared to be textured as a result
of its crystalline nature (rather than as a result of microdim-
ples that might have resulted from ductile failure).
The microanalyses of the brittle phase indicated it to be a
complex carbide. Figure 8 shows pronounced peaks of tita-
nium, tungsten, molybdenum, and titanium, with no peaks of
aluminum or oxygen.
In comparison, spectra from the film (Figure 9) showed
peaks of oxygen, aluminum, and chromium, indicating that
the film was probably an oxide of aluminum and chromium.
However, since nitrogen cannot be easily detected using SEM,
the possibility of the film containing or even being constituted
entirely of nitrides cannot be ruled out. The semiquantitative
Fig. 2—A schematic view of the turbine blade used in this study. The over- spot analyses (Table II) and the line scans (Figure 10) of these
all height was approximately 1 m. two areas of the fracture surface confirm these findings.

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Fig. 3—Cut-up diagram of the turbine blade of Fig. 2 showing the sections for examination.

(a)

(a)

(b)
Fig. 4—(a) Optical and (b) scanning electron micrographs showing a gen-
eral region in the segregated area of the sample (unetched, magnification
100 times).
(b)
Fig. 5—(a) Optical micrograph of a normal area of the sample in areas away
from the defect showing no carbide concentration (unetched, magnification
100 times). (b) The left-hand side of the scanning electron image shows
carbides in the segregated area. The crack is seen to extend into the unseg-
regated region on the right, which appears slightly lighter, and where no
carbides are seen (unetched).

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(a) (b)

Fig. 6—Optical micrographs showing (a) a general area with no carbides and (b) a segregated area with carbides (white areas). Etched.

(a) (b)

(c) (d)

(e)
Fig. 7—Fractographs showing a film associated with the brittle phase in the segregated part of the fracture surface, magnified (a) 50 times, (b) 250 times,
(c) 1000 times, (d) 2000 times, and (e) 8000 times.

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(a) (b)
Fig. 8—(a) A fracture surface showing the brittle phase in the segregated area and the overlying film. (b) A typical EDX pattern of the brittle phase at
point 1 showing predominant peaks of C, Ti, W, and Mo (EDX patterns at points 2 and 3 showed closely similar results).

(a) (b)
Fig. 9—(a) The fracture surface in the segregated region showing a film overlying a brittle phase. (b) A typical EDX pattern of the film at point 4 show-
ing evidence of the presence of oxygen with aluminum and chromium (EDX pattern at point 5 showed a similar result).

Table II. EDX Analysis of Different Areas of the Segregated Region of the Fracture Surface

Spectral Analysis (Wt Pct)

Area of Interest Spectrum Number C O Al Ti Cr Co Ni Mo W Total
Brittle phase spectrum 1 11.96 * * 43.37 2.91 1.24 9.03 11.01 20.48 100.00
spectrum 2 13.14 * * 42.02 3.02 1.25 8.68 11.08 20.82 100.00
spectrum 3 12.57 * * 40.72 2.76 1.65 11.25 10.67 20.39 100.00
Film spectrum 4 4.59 0.47 3.54 4.92 14.17 8.47 54.98 4.45 4.42 100.00
spectrum 5 6.61 0.82 2.94 6.78 12.99 8.18 50.89 5.02 5.77 100.00
*Not detected.

In contrast, the “normal” area (i.e., far from the freckle
defect) of the fractured surface (Figure 11) did not contain
any bright area indicative of the presence of oxide or nitride
films. The carbide particles were smaller and the presence
of oxide (or nitride) film could not generally be detected
in association with the carbides. The EDX pattern and the
analysis of carbides were similar to those obtained from the
carbides found in the freckle area. The matrix pattern
and analysis (Figures 12 and Table III) complied with the
general composition of the alloy. However, one EDX pat-
tern (Figure 13) from this region did show peaks of oxygen
and aluminum, indicating that there were some oxides

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Fig. 10—EDX line scan showing the variation in composition of oxygen, aluminum, and chromium along the line shown in the same image used for spec-
tral analysis.

(a) (b)

(c) (d)
Fig. 11—Typical fractographs showing the general area of the fracture surface away from the segregated region, magnified (a) 50 times, (b) 200 times,
(c) 1000 times, and (d) 2000 times.

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Table III. EDX Analyses from the General (Nonsegregated) Area of the Fracture Surface

Spectral Analysis (Wt Pct)

Area of Interest Spectrum Number C O Al Ti Cr Co Ni Mo W Total
Brittle phase spectrum 1 16.85 * * 39.77 2.18 1.16 8.47 10.15 21.42 100.00
spectrum 4 11.74 * 0.75 33.57 4.41 3.64 25.61 8.38 11.90 100.00
The matrix spectrum 2 2.04 0.37 2.15 3.94 13.76 9.09 63.14 2.66 2.84 100.00
spectrum 3 * * 0.58 2.98 11.48 9.68 72.38 0.92 1.34 100.00
*Not detected.

(a) (a)

(b)
Fig. 12—(a) Fracture surface showing the brittle phase of an area away
from the segregated region, with (b) typical EDX pattern at point 1, show-
ing predominant peaks of C, Ti, W, and Mo (EDX pattern at point 4 showed
a similar result).
(b)
Fig. 13—(a) The fracture surface of the matrix area away from the segre-
gation defect with (b) EDX spectrum at point 2 showing peaks of nickel,
chromium, aluminum, titanium, cobalt, carbon, and oxygen.

embedded in the matrix. Another, Figure 14, appeared to be
pure matrix.
IV. DISCUSSION
Because the channel defect contains heavily segregated
liquid of a low melting point, it solidifies significantly later
than its surroundings, so that the shrinkage accompanying
solidification is not easily fed. The liquid in the channel,
therefore, suffers reduced pressure, so that if the defect is
near the surface of the casting a surface sink may therefore
be drawn inward, explaining the surface depressions that are
widely known to characterize those channels that occur near
or at the casting surface.

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(a)
(b)
Fig. 14—(a) The fracture surface of the matrix area away from the segre-
gation defect, with (b) EDX spectrum at point 3 showing peaks of nickel,
chromium, titanium, and cobalt.
In addition, the reduced pressure will open any bifilms that
happen to be present in the freckle, forming internal cracks.
Bifilms are expected to be present because they will be pushed
ahead of the advancing dendrites.[1] They are pushed because
even if the oxide itself could be assimilated, the dendrite can-
not penetrate the layer of residual air (since our vacuum is,
of course, simply “dilute air” in this case) trapped between
the doubled-over oxide. Thus, bifilms are expected to be con-
centrated in channel segregates.
The occasional extension of a crack into the surrounding
nonsegregated matrix, as seen in Figure 5(b), is understood
if the bifilm extends some way into the matrix, where it has
become trapped between dendrites.
The total length of such cracks is not easily estimated.
The maximum observed length in sections transverse to the
axis of the channel defect was about 2 mm, being approxi-
mately the width of the channel defect in places. However,
the observed length of the channel was at least 25 mm and
could easily be envisaged as being 50 to 100 mm or more
2070—VOLUME 35A, JULY 2004
in total length. Thus, the length of cracks along the channel
might be soberingly long.
The film might be amorphous when first entrained in
the melt, probably during the pour. This is the case in low-
melting-point alloys such as Al-based alloys, where the film
retains its smooth surface appearance and delicate folds.[4]
However, because of the high temperature at which Ni-based
alloys are cast, a smooth, microscopically featureless amor-
phous film would be expected to transform rapidly into a
crystalline form and would probably experience successive
recrystallizations, consistent with the textured appearance at
high magnification seen in Figure 7.
The existence of the carbide on the wetted underside of
the film is again thought to be analogous to the precipitation
of Fe-rich phases[5,6,7] and Sr-rich phases[8] in Al-Si alloys.
In the case of beta-iron intermetallics in the Al-matrix phase,
the phase nucleates and grows on the two wetted outer sur-
faces of bifilms, resulting in the appearance of a platelike
Fe-rich phase with a crack along its center, the crack being
the originating doubled-over film. When subject to tensile
failure, the macroscopic crack seeks out the beta-Fe particles,
following their central bifilm crack. Thus, on a fracture sur-
face, the appearance is that of an oxide film overlying the
intermetallic phase. In the Ni-based alloy, it seems the oxide
film does, in fact, overlie the carbide (Figures 7 through 10),
in agreement with this analogy.
The finding of oxides in regions far from the channel
defect (Figure 13) suggests that the defects are common in
vacuum–melted and cast Ni-based alloys. (The oxide in this
case appears to be yielding a low oxygen signal, diluted by
the signal from the carbides and matrix. The dilution might
reflect its thinness, or it unfavorable orientation.) The defect
seems likely to be an “old” oxide,[1] originating from slow
thickening during the preparation of the alloy at the alloy
manufacturer (in contrast to the “new” and necessarily thin
oxides created during the brief duration of the pouring of
the casting). If, in fact, it is an old oxide, such defects are
better integrated with the matrix, since their layer of air has
had more time to be completely assimilated by the contin-
ued growth of the bifilm (inward in this case, consuming
the residual air in the entrained vacuum). Thus, they are less
effective as initiation sites for porosity or crack formation.
Their appearance, too, is less filmlike, being usually rather
craggy and crystalline.[1] In addition, old oxides are more
likely to be enveloped by the advancing dendrites and incor-
porated into the matrix. Even so, of course, they remain
unwelcome discontinuities in the alloy and are likely to retain
some capability of initiating porosity or cracks in favorable
conditions.
This study has added to the evidence that the turbulent
pouring of Ni-based alloys, even in vacuum, does result in
the entrainment of bifilms. These act as cracks and are expec-
ted to weaken castings in a serious and random fashion.[1]
Development work on the filling of other liquid alloys into
a mold has demonstrated that the surface turbulence during
the pouring of metal can be controlled and by some tech-
niques prevented altogether.[9,10] If means could be devised
for the filling of turbine blades in this way, the potential for
the improved performance of turbine engines might be greatly
enhanced. One can imagine a development that parallels the
massively important advance from flake to spheroidal
graphite cast iron.
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V. CONCLUSIONS
1. During the pouring of liquid metals, if the surface film on
the liquid is a solid phase, it is randomly folded (entrained)
into the liquid metal in the form of double-oxide (and/or
possibly nitride) films (bifilms) that act as cracks. This behav-
ior necessarily follows, because the oxide film is folded dry
side to dry side, so that no bonding across this double oxide
interface is to be expected. They are, therefore, expected to
represent threats to the strength and toughness and the fatigue
and creep lives of cast components. Defects consistent with
such an origin have been shown to be present in vacuum-
cast Ni-based turbine blades for the first time.
2. Large castings are expected to be particularly at risk from
entrainment defects as a result of the height of the pour
and the length of time for pouring, both maximizing the
entrainment action. In addition, the length of time for
solidification will maximize the chance of formation of
freckle defects, the concentration of bifilms, and the open-
ing of bifilms to form internal cracks.
3. Carbides appear to nucleate and grow on the outer, wetted
surfaces of the bifilms. The inner, unbonded interface of
the bifilm gives the carbides the appearance of being cracked
and, therefore, appearing brittle. Growth of second phases
on bifilms, together with the accompanying crack from the
originating bifilm, appears to be common in cast metals.
4. For the future, it is predicted that the manufacture of cast-
ings without bifilms appears, in principle, to be feasible,
promising castings of greatly improved performance and
reliability.
METALLURGICAL AND MATERIALS TRANSACTIONS A
ACKNOWLEDGMENTS
This project has been financially supported by the
Association of Commonwealth Universities and has
benefited from the use of research facilities at the IRC
in Materials Processing and the Department of Metal-
lurgy and Materials of Birmingham University. AKMBR
gratefully acknowledges the one-year study leave from
Bangladesh University of Engineering and Technology
(BUET).
REFERENCES
1. J. Campbell: Castings, 2nd ed., Butterworth Heinemann, Oxford, United
Kingdom, 2003.
2. M. Cox, M. Wickins, J.P. Kuang, R.A. Harding, and J. Campbell:
Mater. Sci. Technol., 2000, vol. 16, pp. 1445-52.
3. M. Cox, M. Wickins, R.A. Harding, and J. Campbell: 1998, unpublished
work, quoted in Ref. 1, p. 61.
4. M. Divandari and J. Campbell: Trans. Am. Foundry Soc., 2001, vol. 109,
pp. 201-12.
5. X. Cao and J. Campbell: Trans. Am. Foundry Soc., 2001, vol. 109,
pp. 269-83.
6. X. Cao and J. Campbell: Metall. Mater. Trans. A, 2003, vol. 34A,
pp. 1409-20.
7. S.G. Shabestari, M. Mahmudi, M. Emamy, and J. Campbell: Int. J.
Cast Met. Res., 2002, vol. 15, pp. 17-24.
8. S.M. Miresmaeili, W.D. Griffiths, J. Campbell, S.G. Shabestari, and
S.M.A. Boutorabi: unpublished research, 2003.
9. J. Campbell: Review: Developments in Filling System Designs, CIATF
Technical Forum, Stratford, United Kingdom, June 1997.
10. J. Campbell: Castings Practice, Butterworth Heinemann, Oxford, United
Kingdom, 2004.
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