International Journal of Engineering and Natural Sciences (IJENS’s), Vol. 1, Num.

Failure Analysis of Jet Turbine Engine High Pressure Nozzle

Material Made of Cobalt Based Super Alloy
Ozan Çoban, Özgür C. Arslan, and Tuba Karahan

Metallurgical and Materials Engineering Department, Istanbul Gedik University

Kartal Campus, Kartal/Istanbul, 34876, Turkey
[email protected]; [email protected]; [email protected]

Received: 27.11.2018 Accepted: 24.12.2018

Abstract: In this study, we carried out the failure analysis based on metallographic research of a cobalt superalloy material which
had been used in jet turbine engine. The failure analysis was made by chemical composition analysis, hardness test and
microstructural researches after metallographic sample preparation on the material which had operated about 30000 hours and
damaged. Macro cracks which can be seen by visual inspection have been detected on the cobalt based superalloy nozzle
material’s some surfaces which had exposed to high temperature and high pressure fuel-air mixture. After the metallographic
sample preparation and optical and electron microscope investigation, it has been determined that the main reason of the failure is
coarse and continuous morphology M7C3 carbide precipitations on the grain boundaries and as a result of that, stress corrosion
cracking has moved through that grain boundaries which have been embrittled and weakened against high temperature corrosion.
Also, after consideration of the chemical composition on the damaged area of material, it has been detected that, owing to the
usage of carbon content fuel during operation, carbon diffusion at high temperature into the material had occurred. So, with high
carbon content in the material, the type and morphology of the carbides had changed and caused the failure.

Keywords: Failure analysis, jet engine and turbine, nozzle, cobalt base superalloy, carbide transformation, stress corrosion,
microstructure, optical microscopy.

1. INTRODUCTION superalloys is their microstructures. The microstructures of

these materials might be changed during the operation
Nickel and cobalt based superalloys are the materials because of high temperatures. The phases in the
which have been widely used in both aerospace industry and microstructure, morphologies of them and the regional
also gas turbines. Their excellent creep resistance, high chemical compositions can be changed. Therefore, the
temperature corrosion resistance and also having higher failure analysis is carried out in the foreseen lifetime of the
strength at elevated temperatures make cobalt based super material and reparation or renewal decision is made
alloys more profitable in comparison with nickel based according to the analysis. The basic method for failure
superalloys [1]. In this sense, cobalt based superalloys are analysis of these type of cobalt based superalloys is
widely used in some critical parts of jet engines. One of metallography. The sample prepared by metallographic
these critical materials is high temperature nozzle. The task sample preparation processes is subjected to the optical
of this material which is used as first stage high pressure microscopy and/or electron microscopy investigation. As a
nozzle in jet engines and power turbines is conveying the result of microscopic investigation acting like a detective
hot gas flow that released from the combustion chamber searching a crime, according to the failure or crack structure
most efficiently and with best angle through the rotating and according to the phase changes in the microstructure of
parts of turbine. Therefore, more than mechanical stresses, material, the failure mechanism is determined.
this nozzle is exposed to thermal loadings and also bending The aim of that study is to determine the reason of the
stresses due to the gasses which have high temperature and failure on the first stage high pressure nozzle material which
pressure. In this case, the possible material failure had operated approximately 30,000 hours while it had been
mechanisms which can be occurred during these operation predicted to operate for 70,000 hours. In addition to that,
conditions are creep, creep-fatigue, thermal fatigue, another aim of that study is to determine the correct
oxidation and high temperature corrosion [2]. metallographic sample preparation processes of cobalt
The most important factor that determines the based superalloys. By carrying out optical microscopy and
performance of the nozzles made of cobalt based electron microscopy investigations, determination of the

Copyright © IJENS’s. All rights reserved. 13

 Çoban, O. et al., (2018), Failure Analysis of Jet Turbine Engine High Pressure Nozzle Material
Made of Cobalt Based Super Alloy
failure mechanism on the nozzle and according to the 2.2. Hot Molding
results, improving the service life of the material are the
main targets of that study. Hot molding method was preferred in order to both make
cut parts hand-held and inserted into neatness for all next
2. MATERIALS AND METHODS steps which are grinding-polishing, etching and microscopy.
Ecopress 50 Hot Molding Machine and bakalite and acrylic
The material on which failure analysis has been carried powders were used for molding process. The temperature
out is a cobalt based superalloy which had operated for was 1900C, the pressure was 130 bar and the duration was 3
30,000 hours inside the General Electric CF6-50 high by- minutes for sintering and 3 minutes for cooling.
pass turbofan engine as first stage high pressure conveying
nozzle and it has been shown on Figure 1. 2.3. Grinding – Polishing

After molding, grinding and polishing processes were

applied to the samples by Metkon Forcipol 2V machine
which is located in Istanbul Gedik University Metallurgical
and Materials Engineering Laboratory. SiC grinding disks
were used as abrasives during grinding process. The
rotational speed was 300 rpm during both grinding and
polishing. For polishing, 0.25 µm mono crystalline diamond
suspension and diamond based lubricant were used.

2.4. Etching

For microstructural analysis with optical microscope;

from optic physics and inorganics chemistry aspects, the
requirement is creating metallurgical contrast on the surface
Figure 1. First stage high pressure nozzle to be investigated. In order to actualize it, a chemical called
etchant is used.
2.1. Sampling In order to carry out optical microscopy investigation,
etching process was applied to the polished samples with
After visual inspection, sampling was carried out from convenient etchants and in optimum etching durations. We
the macro crack zones and also non-damaged parts for applied the both chemical etching and electrolytic etching
comparison. The sampling zones of the sample and the methods.
names of zones were shown on Figure 2. For chemical etching, Kallings No:2 etchant was
prepared with 5 gr CuCl2, 100 ml hydrochloric acid (HCl)
and 100 ml ethyl alcohol (ethanol). For electrolytic etching,
a solution which includes 10 ml HCl, 10 gr CrO3 and 100 ml
distilled water was prepared. The sample was attached to
the positive pole of a direct current power supply as anode
and 304 stainless steel as cathode to the negative pole. Both
anode and cathode were submerged into the etchant solution
and 6 V voltage has been applied for 10 seconds duration.
Immediately after etching, the sample was washed
thoroughly with ethyl alcohol and water and dried with
warm air flow.

2.5. Microstructural Investigation

Figure 2. Sampling zones After the sample was etched in correct duration and
correct etchant, the metallurgical phases were dissolved in
The cutting process for sampling step of metallography different amounts from the aspect of electrochemistry, in
was carried out by using Metacut 251 abrasive cutting micro scale. And the phases reflected the light
machine which has SiC cutter disk and liquid cooling characteristically due to their spectrum difference of each.
system in Istanbul Gedik University Metallurgical and We could see the microstructure of the cobalt based
Materials Engineering Laboratory. superalloy, which had been damaged in micro and also
macro scale, by using BAB Software Optical Microscope.

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For physical structural investigation and chemical that the material is cobalt based superalloy and the chemical
composition investigation of critical parts of micro crack, content values are approximate with the values of FSX 414.
we used EDS equipped High Vacuum 20 kV scanning
electron microscope which is located in Yalova University Table 1. Chemical analysis result
Laboratory.
Element % by weight Element % by weight
2.6. Chemical Analysis and Hardness Test Ni 23.8425 Ti 0.4329
C 0.2080 Co 42.0733
For failure analysis of nozzle sample, beside the
metallographic characterization, also chemical analysis and W 6.3959 Cr 22.6896
hardness tests were carried out by XRF Spectrometer,
Mo 0.3453 Si 0.9519
Carbon-Sulphur Analyser and Digirock HV30 Vickers
Hardness Testing Machine in Gedik Holding Research and Fe 0.4794 Ta 0.8566
Development Laboratory and Gedik Test Center. 1.4629 0.2617
Al Others
3. RESULTS AND DISCUSSIONS
Before the microstructural analysis, hardness tests were
As the first step for failure analysis of the sample which carried out on different points which have particular
had operated for 30,000 hours in turbine engine combustion distance to macro crack center line. Hardness test results
chamber, visual inspection was carried out and macro have been shown on Figure 4. Hardness values are
fractures and macro cracks were detected on outer surface approximate to each other in macro scale. Therefore, it was
as shown on Figure 3. thought that locational hardening due to heat treatment
effect or softening due to grain size growth should not have
been occurred on the microstructure.

Figure 4. Hardness test result

Figure 3. Failure zone detected by visual inspection
After hardness tests, metallographic sample preparation
As the result of visual inspection, 2 main fracture failures and optical microscope investigation were carried out and
and 1 macro crack failure were detected. The failure has as results, the microstructures below were obtained.
occurred on a zone on which hot and high pressure gas According to these microstructures;
might have been circulated and which is close to the
connection zone with the platform. Both high temperature
and pressured gas were existed around that zone and also
stresses might have occurred on it. For that reason, it has
been thought that the failure mechanism would be a stress-
corrosion cracking.
After visual inspection, we decided to carry out optical
microscopy investigations on the surface around the macro
crack. Macro crack could give us some predictions about
the reason of failure because it can represent the main
fracture failures.
Before metallographic sample preparation and
microstructure analysis processes, chemical composition
analysis was carried out on the sample which had been
taken far from the failure zone. According to the XRF
elemental analysis result given on Table 1, it could be seen Figure 5. Microstructure of macro crack zone (100x –
electrolytic etched with 6% chromic acid + 10% HCl)

Copyright © IJENS’s. All rights reserved. 15

 Çoban, O. et al., (2018), Failure Analysis of Jet Turbine Engine High Pressure Nozzle Material
Made of Cobalt Based Super Alloy
On Figure 6, the microstructure of the area that macro The microstructure obtained from zone 2 but far from the
crack had occurred and propagated through has been given. main fractures and macro crack has been given on Figure 7.
When we looked at the structure of the crack, we thought It can be seen on microstructure that spherical and chain
that macro crack could have occurred by growth of type carbides have precipitated on the grain boundaries.
intergranular micro cracks. In order to understand the However it has been detected that, the morphologies of
mechanism of failure, first, microstructural investigation of carbides are changing by approaching to the macro crack.
non-damaged zone was carried out. On Figure 6, the When the microstructure, obtained from closer point to
microstructure taken from zone 3 has been given. macrocrack, given on Figure 8 is considered, it can be seen
that some of the spherical and chain type carbides, are
replaced by continuous formed carbides.

Figure 6. Microstructure of cobalt based superalloy (100x –

electrolytic etched with 6% chromic acid + 10% HCl)

Twinnings inside the austenitic matrix of face centered

cubic (FCC) structure and also carbide precipitations on
grain boundaries and inside the grain can be seen on the
microstructure that given on Figure 6. The transformation of Figure 8. Microstructure of carbides obtained from closer
lattice structure from face centered cubic (FCC) to zone to macrocrack (100x - electrolytic etched with 6%
hexagonal closed pack (HSP) structure occurs on cobalt chromic acid + 10% HCl)
based superalloys over 4170C. In order to avoid this
transition, cobalt based superalloys are alloyed with nickel When we get closer to the macro crack, it can be seen
[3]. Because our material includes nickel over than 10 %, it that the amount of continuous formed carbides are
could be understood that the lattice structure of the matrix is increasing as shown on the microstructure that given on
FCC. The basic phases that affect the mechanical properties Figure 9.
of cobalt based superalloys are the carbide phases.
Therefore, the microstructures of carbides have been
investigated and the results were obtained as;

Figure 7. Microstructure of carbides obtained from non- Figure 9. Microstructure of carbides near the macrocrack
damaged zone (100x - electrolytic etched with 6% chromic (200x - electrolytic etched with 6% chromic acid + 10%
acid + 10% HCl) HCl)

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Lamellar morphology carbides and continuous formed

carbides precipitated on grain boundaries and also other
types of carbides and leaves phases inside the grains can be
seen on the microstructure given on Figure 9.
After the detection of carbide morphology changes
through the macrocrack, we decided to investigate the
origin, sides and tip of the macrocrack and the
microstructures are;

Figure 12. Microstructure of the tip zone of crack (200x

slightly chemically etched with Kallings No:2)

Figure 10. Microstructure of macrocrack origin (100x –

slightly chemically etched with Kallings No:2)

Microstructure of macrocrack origin zone, which had

been slightly chemically etched, has been given on Figure
10. Due to the fact that oxides are electrochemically
affected by etchants more than metallic phases, it has been
thought that the brown colored parts surrounding the crack
could be hot corrosion products. After that estimation, we
decided to carry out electrolytic etching.

Figure 13. Microstructure of the tip zone of crack (100x -

electrolytic etched with 6% chromic acid + 10% HCl)

As it can be seen on Figure 12 and Figure 13 which

shows the microstructure of tip zone, macrocrack has
propagated up to a point and then it continued as micro
crack on its path passing through the continuous formed
carbides that have precipitated on the grain boundaries as it
can also be seen on Figure 14 which shows the
microstructure of micro crack tip. It can also be seen that
microcrack propagation stops and possibly nanocracks
Figure 11. Microstructure of macrocrack origin (100x – propagation occurs up to lamellar morphology carbides
electrolytic etched with 6% chromic acid + 10% HCl) which have also precipitated on grain boundaries.
On the microstructure of macrocrack zone has been given
on Figure 11, intergranular corrosion cracks and continuous
carbides on grain boundaries could be seen. After that we
decided to investigate the tip zone of the crack in order to
see propagation mechanism of it.

Copyright © IJENS’s. All rights reserved. 17

 Çoban, O. et al., (2018), Failure Analysis of Jet Turbine Engine High Pressure Nozzle Material
Made of Cobalt Based Super Alloy

Figure 14. Microstructure of microcrack tip (200x -

electrolytic etched with 6% chromic acid + 10% HCl)

After optical microscopy analysis we considered the

results and decided to carry out electron microscope Figure 17. SEM image of microcrack
analysis in order to determine the types of carbides
chemically and morphologically. On the Figure 15 and In cobalt based superalloys, M23C6 and M7C3 carbides
Figure 16, SEM images of crack zone have been shown. It form during the last stage of solidification and the carbide
can be seen that macrocrack had propagated mostly through type is basically related to Cr/C ratio. While M7C3 carbides
grain boundaries zone. And also corrosion products can be occur at lower Cr/C ratio, M23C6 carbides occur at higher
seen around the macrocrack. Cr/C ratio [4].
SEM-EDS analysis was carried out on the points shown
by blue rectangles on Figure 18. According to the results
given on Table 2, continuous carbides include higher
carbon and lower wolfram and molybdenum in comparison
with lamellar carbides. When we compare the Cr/C ratios,
while the ratio of continuous carbide is 2.012, the ratio of
lamellar carbide is 2.904. As the result of SEM-EDS
analysis, it could be understood that lamellar carbides are
M23C6 and continuous carbides are M7C3.

Figure 15. SEM image of macrocrack

As shown on the SEM image of macrocrack tip zone on

Figure 16, macro crack propagation is blocked by semi
lamellar semi continuous morphology carbide precipitates.
However, macrocrack had found a path for propagation as
microcrack. As it can be seen on Figure 17, the path of
microcrack is surrounded by continuous morphology
carbides. It means that microcrack had propagated through
the continuous carbides on grain boundaries. Figure 18. SEM-EDS image of carbides

Table 2. SEM-EDS analysis results

Ta
C% Mo% Cr% Co % Ni % W%
%
Lamellar 53,1
18,31 6,97 8,97 1,48 1,57 9,52
Carbide 8
Continuou 55,1
27,32 1,72 7,52 1,06 1,6 5,63
s Carbide 5

In super alloys, dense and continuous carbides expedite

crack occurrence and propagation, decrease ductility and
toughness by 30 % and shorten the lifetime of the material
Figure 16. SEM image of macrocrack tip zone [5]. This could be seen on this study, too. As it can be seen
on the microstructures obtained by both optical microscopy

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and electron microscopy investigations, the failure that had occurrence of M6C carbides and M6C carbide occurrence
occurred on the nozzle, the macrocrack and microcrack, had can decrease the potential of M7C3 carbide occurrence. In
propagated through M7C3 type continuous carbides and the addition, as it can be indicated with (2), these elements
propagation had been blocked or slowed down by M 23C6 increase the possibility of carbide transformation from M 7C3
type lamellar carbides. to M23C6. Thus, these alloying elements could help to obtain
more ductile carbides on the grain boundaries and could
Table 3. Carbide types in cobalt based superalloys [6] prevent grain boundary embrittlement. So, increasing Mo
and W alloying elements could increase the lifetime of a
Carbide Elements Morphology
Type
cobalt based superalloy nozzle which operates under these
MC Ti, Nb, Zr, Hf, Ta Spherical, cubic or kinds of conditions like exposing carbon diffusion from the
disordered shaped as hot gas which includes unburnt carbon.
particles and shinny
M7C3 Cr As blocks, continuous 3Cr7C3 + 2 (Mo,W) = Cr21(W,Mo)2C6 + 3C (2)
formed and extends
through grain boundaries According to the carbide transformations during the
M23C6 Cr, W Spherical, layered or service according to the (1) and (2), beside the wolfram and
lamellar morphology and molybdenum content increase advisory for solution, also the
on grain boundaries
content of MC type carbide making elements could be
M6C Mo, W Randomly dispersed,
pinkish white
increased in order to minimize the M23C6  M7C3
transformation due to high chromium activity. Owing to
both carbonization due to diffusion and also carbon
The carbide types that occur in cobalt based superalloys
occurrence due to transformations, instead of carbon’s
are given on Table 3. The mole ratio of carbon,
making brittle continuous Cr7C3 carbides on grain
corresponding to 1 mole of metal, decreases when descend
boundaries, MC type carbides such as TiC, NbC, TaC could
through the below of the table. In other words, in the
be provided to be occurred inside the grain.
presence of these elements, the amount or the possibility of
The elements, advised to be increased in cobalt based
formation of upper side carbides increases with the increase
super alloy which is to be used as first stage high pressure
of carbon content.
nozzle in a jet turbine engine, in a sense, would replace with
chromium and owing to this we could provide both high
Cr23C6 + 3C = 3Cr7C3 + 2Cr (1)
stress corrosion resistance and also could increase the high
temperature corrosion resistance. Because in the presence of
As it can be indicated with (1), when the carbon content
these elements, instead of brittle Cr7C3 carbides, more
increases, carbide formation can occur and beside the
ductile Cr21(W,Mo)2C6 carbides would occur on grain
lamellar M23C6 type carbides (Cr23C6 and W23C6),
boundaries and also it can be provided that chromium
continuous M7C3 type carbides (Cr7C3) precipitate on grain
would make Cr2O3 layers, which increases the corrosion
boundaries. After that consideration, in order to see if there
resistance, instead of making carbides.
were any carbon content difference between the non-
damaged parts and damaged part of the nozzle, we decided
4. CONCLUSION
to carry out carbon - sulphur analysis to the sample, which
has been taken from the part of the nozzle on which
macrocrack had occurred. According to the C-S analysis The cobalt based super alloy sample; which had been used
results, strikingly, while non-damaged part of the nozzle as nozzle for conveying the hot and high pressure air-fuel
includes 0.2 % carbon, the part of the nozzle on which mixture, released from combustion chamber, through first
failure occurred includes 0.4 % carbon. As the result of stage high pressure turbine; could have operated 30,000
carbon analysis, it can be claimed that because of carbon hours while it had been estimated to operate 50,000-70,000
diffusion into the part of the nozzle from hot gas including hours because of failure. In our failure analysis study, we
unburnt carbon, the carbon content of microstructure had detected the reason of the failure as carbide transformation
increased and carbide transformation (M23C6  M7C3) had due to carbon diffusion on to the material from circulated
occurred. gas which might have included unburnt carbon. Related to
In all super alloys, carbides are the weak phases against the carbon diffusion, because of M23C6  M7C3 carbide
oxidation. In order to minimize the high temperature transformation, the grain boundaries had embrittled and
corrosion failure, carbides need to be small and weakened against stress corrosion crack propagation due to
discontinuous [7]. When all the microstructures are the fact that continuous formed brittle M7C3 carbides are
considered in our study, it can clearly be seen that the crack acting like a pathway for crack propagation while lamellar
had propagated through continuous morphology carbides. In formed ductile M23C6 carbides are acting like a block.
order to avoid this occurrence, the carbide transformation We also estimated that the lifetime of the nozzle could be
needs to be blocked. As a resolution advisory, molybdenum increased by preventing carbide transformation by
and/or wolfram contents could be increased in order to increasing the molybdenum and wolfram content of the
succeed it. These elements increase the potential of material, because they increase the possibility of M23C6

Copyright © IJENS’s. All rights reserved. 19

 Çoban, O. et al., (2018), Failure Analysis of Jet Turbine Engine High Pressure Nozzle Material
Made of Cobalt Based Super Alloy
carbide occurrence at elevated temperatures despite carbon
diffusion during service. In addition to molybdenum and
wolfram content increasing advisory, we also estimated that
increasing MC carbide making alloying elements content
such as Ti, Nb, Ta and Hf could be beneficial for cobalt
based superalloys which operate at high temperatures and
under the conditions of carbon diffusion might be occurred.
Space and aerospace industry are continually developing
engineering application industries. At that point, material
failures should be minimized for these kinds of critical parts
such jet engine parts. In order to minimize the failures,
failure analysis studies should be increased and developed.

ACKNOWLEDGMENT

First and foremost, we give special sincerest gratitude to

Prof. Dr. Muzeyyen Marsoglu for her psychological and
scientific supports and Prof. Dr. Ahmet Topuz and Prof. Dr.
Sunullah Ozbek for their support on the study. In addition,
we would like to thank Gedik Holding Research and
Development Department and Gedik Test Center for
chemical analysis and mechanical tests and also Yalova
University for electron microscopy analysis.

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