Doc.

X- 1639 - 08
FAILURE ANALYSIS OF HP STEAM SUPERHEATER
AT A FERTILIZER PLANT
A. El-Batahgy*, H. Abu-Zamil** and H. Assaad**
* Head of Manufacturing Technology Department, Central Metallurgical
R & D Institute, Cairo, Egypt
** Inspection Sector, Abu-Qir Fertilizers & Chemical Industries Company,
Alexandria, Egypt

Abstract
After 21 years of operation, both header and tubes of superheater were failed
due to creep damage accelerated by long-term overheating. Creep damage was
accumulated as a result of metallurgical instability including decomposition of
pearlite into ferrite and spheroidized carbide particles that caused severe
embrittlement and initiation of voids, intergranular micro-cracks, and separation
of grains. Such metallurgical instability could be accelerated with overheating
that in turn reduce creep lifetime.
Long-term overheating was evident from existence of adhesive, thick scale
layer with little or no detectable change in the tube wall thickness. Long-term
overheating of header was occurred as a result of plugging of 10 tubes, located
beside each other in the same zone.
Ruptured header was replaced with new one while ruptured tube was plugged
and boiler was set into normal operation as a temporary solution. Then, it was
decided that non-failed superheater' tubes will be subjected to detailed
investigations including non-destructive and destructive tests to evaluate its
condition during the nearest normal shut down. Based on such investigations, it
will be decided if other non-failed tubes of the superheater are still safe to be
used under the working conditions or if it will be about to be replaced with new
tubes.
In order to decrease the possibility of such failure in future, the operation
conditions should be restrictly controlled to avoid overeating and then, to
increase the lifetime of superheater tubes. Besides, periodic maintenance for
checking and evaluating of superheater condition using different nondestructive inspection techniques then, carrying out necessary repair works is of
considerable importance. During such periodic maintenance, removal of scale
from boiler tubes is recommended in order to avoid overheating of tubes. In this
regard, chemical or mechanical cleaning of tubes can be applied.
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Doc. X- 1639 - 08
1. Background
The subject HP steam superheater has been set into service 21 years ago. In this
superheater, the heat of flue gases (collected from both boiler and reformer) is
utilized for superheating the saturated steam leaving the steam drum after being
produced from the boiler. The high pressure steam produced serves primarily
for driving the turbines for power generation. The superheater includes a total of
162 U-bends seamless tubes (54 rows x 3 tubes) fixed in a horizontal position
where length of superheater tube bundle is 7160mm. Direction of the heating
flue gases is a perpendicular to the axial direction of tubes, with its flow from
steam outlet header side to steam inlet header side.
Superheater tubes were made from 15Mo3 steel (DIN Standard) with 38mm
nominal diameter and 4.0mm wall thickness. Both inlet and outlet headers were
made from 15Mo3 steel (DIN Standard) with 298.5mm nominal diameter and
27.5mm wall thickness. Inlet and outlet temperatures of superheater steam are
328C and 410C respectively while working pressure of superheater tubes is
120bar. Temperature of flue gases outside superheater tubes is approximately
615C.
During the last two years, 10 tubes have been plugged after being leaked. All of
plugged tubes were located just beside each other, within the first 4 rows of
tubes, and its rupture zone was confined to steam outlet header side.
About 9 months later after plugging these tubes, steam outlet header has failed
due to through thickness cracking of its zone at which 10 tubes were previously
plugged. Superheater was shut down and repair has been carried out. In this
regard, the header cracked zone, that included 4 rows of plugged tubes was
removed and replaced with new part having same diameter, thickness and steel
type of header. Since tubes of the new header part will not be used again, the
new header part was made without holes or nozzles for tubes connection. Then,
superheater has been reset into normal operation.
Recently, catastrophic failure of another superheater tube took place, just beside
tubes' supporter zone that is located about 4-5m away from outlet header and
away enough from circumferential tube weld. This fractured tube was located in
the fifth row, just beside outlet header' part that was replaced 9 months ago.
Sample from the failed tube including ruptured zone together with header part
that was previously cracked and removed 9 months ago were subjected to
failure analysis investigations.

Doc. X- 1639 - 08
2. Failure of Steam Outlet' Header
2.1. Non Destructive Examination
The failed header zone was carefully examined before sectioning it for
destructive investigations. General and enlarged views of both ruptured and
non-ruptured samples of failed header are shown in Fig. 1. Visual investigation
showed through-thickness, longitudinal cracking with wider width at header'
outer surface particularly beside seam weld of nozzles with header. This
indicates that cracking was started beside seam weld of tubes' nozzles on
header' outer surface then, propagated through base metal. No thinning or
bulging was observed at header' ruptured zone. The results of wall thickness
measurements showed no remarkable difference in wall thickness of both
ruptured (30.8mm) and non-rupture (31.9mm) zones. It should be reported that
no indications for corrosion or other excessive wastage were observed.
Generally, spite of high operation temperature, visual inspection of ruptured
header showed brittle fracture surface. Except header' ruptured zone, dye
penetrant test showed no indications for other surface cracks either around or
away from ruptured zone.
2.2. Destructive Examination
Specimens from ruptured and non-ruptured zones of header were cut out and
prepared for chemical analysis, metallographic investigations, and hardness
measurements. Results of chemical analysis of ruptured header together with
the specified range for DIN 15Mo3 steel type are shown in Table 1. It is clear
that chemical composition of the ruptured header lies within the specified range
of type 15Mo3 steel.
As-polished stereoscopic and etched optical photographs of a cross section
taken at front of cracked or ruptured zone of header are shown in Fig. 2. The
most important notice is the non-continuous cracks indicating multiple cracks
initiation sites. Optical microscopic investigation confirmed that cracks were
initiated at header outer surface. Higher magnifications of a cross section taken
at front of cracked or ruptured zone of header indicated that cracks were
propagated through grain boundaries voids.
Optical micrographs with different magnifications of a cross section taken from
header' ruptured zone are shown in Fig. 3 while those of a cross section of nonruptured zone are shown in Fig. 4. It is clear that no difference in
microstructures of both ruptured and non-ruptured zones was obtained.
Microstructure of both zones exhibited decomposition of pearlite into ferrite and
spheroidal carbides. Another important notice is the formation of isolated voids
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at outer surface, mid-wall thickness and inner surface of both ruptured and nonruptured zones. Formation of voids has been confirmed by hardness
measurements where lower hardness value (~113HV) was obtained at voids
compared with about 153HV for matrix.
Change or deterioration in microstructure has been confirmed using scanning
electron microscopy as shown in Fig. 5. Scanning electron microscopic
examination has confirmed decomposition of pearlite into ferrite and
spheroidized carbide particles in addition to formation of voids particularly, on
grain boundaries of both ruptured and non-ruptured zones.
Survey of hardness measurements through header' wall thickness of both
ruptured and non-ruptured zones was carried out and the results are shown in
Table 2. The given values are the average of five readings. Results indicated
almost no difference in hardness values of both inner and outer surfaces of
header. However, higher hardness value was obtained at ruptured zone (160HV)
compared with 137HV for non-ruptured zone.
It can be deduced that the microstructure obtained at both ruptured and nonruptured zones is completely different from the original microstructure of
15Mo3 steel that is expected to be ferrite-pearlite structure with lamellar
pearlite phase.
In order to help in identification of failure mechanism, header' rupture surface
was examined using scanning electron microscope as shown in Fig. 6. The most
important notice is the existence of large amount of voids, separation of grains
and the brittle-fracture mode.
3. Failure of Tube
3.1. Non Destructive Examination
The superheater' failed tube zone was carefully examined before sectioning it
for destructive investigations. General views of ruptured tube before and after
removing it out of superheater are shown in Fig. 7. Fracture zone of the
superheater tube was located just beside the supporter of the tubes (Fig. 7-a),
about 4-5m away from outlet header. Visual examination showed tube bulging
at fracture initiation zone and fish-mouth shape rupture with no indication for
corrosion or other excessive wastage. Thickness measurements indicated that
wall thickness was reduced from 4.1mm at non-bulged zone to about 3.3mm at
bulged zone.
Another important notice is the existence of adhesive scale layer, with some
exfoliation, on both external and internal surfaces of fracture zone (Fig. 7-c, d).
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Except fractured or ruptured zone, dye penetrant examination revealed no
surface cracks around or away from ruptured zone.
Stereoscopic examination confirmed exfoliation and cracking of thick adhesive
scale layer formed on outer surface of fracture zone (Fig. 8). It also confirmed
exfoliation and cracking of thick adhesive scale layer formed on inner surface of
fracture zone (Fig. 9). Cracking and exfoliation of this scale layer could be
attributed to tube expansion and contraction due to thermal stresses. Generally,
fracture zone exhibited thick-wall rupture indicating brittle fracture appearance
as shown in Fig. 9-d.
In order to identify the nature of scale layer formed on tube internal and external
surfaces, X-ray diffraction (XRD) technique has been used. The result of this
analysis showed that the formed scale layer consists mainly of iron oxide or
magnetite (Fe304) as shown in Fig. 10.
3.2. Destructive Examination
Specimens from both ruptured and non-ruptured zones were cut out and
prepared for chemical analysis, metallographic investigations, and hardness
measurements. Results of chemical analysis of the ruptured tube together with
the specified range for DIN 15Mo3 steel' type, are shown in Table 1. It is clear
that chemical composition of the ruptured tube lies within the specified range of
DIN 15Mo3 steel.
Regarding metallographic examinations, optical micrographs with different
magnifications of a cross section taken from rupture zone are shown in Fig. 11.
Optical micrographs with different magnifications of a cross section taken from
non-ruptured zone are shown in Fig. 12.
It is obvious that no difference in microstructures of both ruptured and nonruptured zones was obtained. Microstructure of both zones exhibited complete
decomposition of pearlite into ferrite and spheroidal carbides. Another
important notice is the formation of isolated voids at outer surface, mid-wall
thickness and inner surface of both ruptured and non-ruptured zones. Formation
of voids has been confirmed by hardness measurements where lower hardness
value (~111HV) was obtained at voids compared with about 150HV for matrix.
Change or deterioration in microstructure has been confirmed using scanning
electron microscopy as shown in Fig. 13. Scanning electron microscopic
examination has confirmed complete decomposition of pearlite into ferrite and
spheroidized carbide particles in addition to formation of grain boundary' voids
and grains separation at both ruptured and non-ruptured zones.
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Doc. X- 1639 - 08
Survey of hardness measurements through tube' wall thickness of both ruptured
and non-ruptured zones was carried out and the results are shown in Table 3.
The given values are the average of five readings. Results indicated almost no
difference in hardness values of both inner and outer surfaces of tube. However,
higher hardness value (152HV) was obtained at ruptured zone compared with
143HV for non-ruptured zone.
It is obvious that the microstructure obtained for both ruptured and non-ruptured
zones is again completely different from the original microstructure of 15Mo3
steel, which is expected to be ferrite-pearlite structure with lamellar pearlite
morphology.
In order to help in identification of failure mechanism, superheater tube' rupture
surface was examined using scanning electron microscope as shown in Fig. 14.
The most important notice is the existence of large amount of voids, grains
separation and the brittle fracture mode.
4. Discussion
Results of chemical analysis of failed header and tube revealed that its chemical
composition is conformed to that of DIN 15Mo3 steel. Visual investigation of
ruptured header showed through-thickness, longitudinal cracking with wider
width on header' outer surface. It is noticed that cracking was started beside
seam weld of tubes' nozzles on header' outer surface then, propagated through
base metal. Visual investigation showed also brittle fracture appearance where
no thinning or bulging was observed at header' ruptured zone.
Regarding ruptured tube, visual examination showed bulging at fracture
initiation zone and fish-mouth rupture shape with no remarkable thinning,
indicating brittle fracture. Adhesive thick scale layer, with some exfoliation and
cracking was observed on both internal and external surfaces of tube' fracture
zone.
Optical and scanning electron microscopic examinations showed decomposition
of pearlite and forming of grain boundary voids and micro-cracks in addition to
grains separation.
These findings support creep damage accelerated by overheating as failure
mechanism. Creep damage is the result of permanent plastic deformation at
elevated temperatures and at stresses much less than the high temperature yield
stress. Creep damage due to overheating is evident from decomposition of
pearlite and forming of grain boundary voids and micro-cracks in addition to
grains separation. Severe deformation at grain boundaries, together with
diffusion processes can lead to the nucleation and coalescence of voids, causing
separation of grain boundaries.
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In other words, such deterioration in microstructure could result in weakening
of header and tube materials that in turn will result in increase in superheater
pressure above the maximum safe working pressure, which could lead finally to
the current failure or rupture. This means that the properties of the materials of
both header and tube have changed from its original values with respect to the
design values due to the effect of the prolong overheating. Therefore, the
original design values are no longer valid and the materials of both header and
tube failed in a premature manner.
Overheating failures are often classified as either short-term or long term. Shortterm overheating frequently exhibits a thin-lipped longitudinal rupture,
accompanied by noticeable tube bulging, absence of large amounts of thermally
formed magnetite, and violent rupture (sometimes bending the tube almost
double and causing secondary metal tearing) and these are not the features of
the subject case. Long-term overheating usually occurs in superheaters as a
result of different factors including gradual accumulation of adhesive, thick
scale layer and excessive heat input. Internal and external thermal oxidation of
the tube metal is often observed at long-term failure region. In other words,
long-term failures by creep damage can occur with little or no detectable
changes in the tube wall thickness. Microstructural examination is an effective
means of confirming long-term overheating. The platelets of iron carbide in the
pearlite structure of carbon steels will thermally decompose to spheroidized iron
carbide (1-3).
It can be estimated that both header and tube' rupture zones were exposed to
long-term overheating (4-6). It is believed that overheating of header was
occurred as a result of plugging of 10 tubes which were located just beside each
other in the same zone that included the first 4 rows of tubes. Plugging of these
tubes during the last 2 years could lead to long-term overheating of outlet
header particularly, with higher temperature of flue gases on outlet header side
in comparison with inlet header side.
On the other hand, overheating of tube is related mainly to restricted flue gases
around tubes' supporter and forming of thick adhesive scale layer (magnetite;
Fe3O4) on tube surface that in turn will lead to decrease in heat transfer rate. It is
expected that tendency for forming such scale layer is higher at tube outlet side
due to higher temperature than that of tube inlet side. Since magnetite has a
lower thermal conductivity than the steel tube, the net effect is an increase in
tube metal temperature that in turn accelerates creep damage (1).

Doc. X- 1639 - 08
Conclusion and Recommendations
Based on the results of this investigation, it can be concluded that failure of the
subject superheater' header and tube is attributed mainly to creep damage
accelerated by long-term overheating.
It is believed that creep damage was occurred as a result of metallurgical
instability including decomposition of pearlite into ferrite and spheroidized
carbide particles that caused severe embrittlement and initiation of voids,
intergranular micro-cracks, and separation of grains (typical characteristic of
creep failure). Such metallurgical instability could be accelerated with
increasing temperature (overheating) that in turn reduce creep lifetime.
In this failure case, long-term overheating of header was occurred as a result of
plugging of 10 tubes which were located just beside each other in the same zone
that included the first 4 rows of tubes. Plugging of these tubes during the last 2
years could lead to long-term overheating of outlet header particularly, with
higher temperature of flue gases on outlet header side in comparison with inlet
header side.
On the other hand, long-term overheating of tube could be related to restricted
flue gases around tubes' supporter and forming of adhesive magnetite scale
layer on tube internal surface that acts as a barrier to heat transfer. It is expected
that tendency for forming such scale layer is higher at tube outlet side due to
higher temperature than that of tube inlet side. Since adhesive magnetite scale
layer (up to 0.4mm) has a lower thermal conductivity than the steel tube, the net
effect is an increase in tube metal temperature that in turn accelerates creep
damage as a result of change or deterioration of microstructure.
As a temporary solution, ruptured tube was plugged and superheater was reset
into service. At the same time, decision was made to subject non-failed
superheater' tubes to detailed investigations including different non-destructive
and destructive tests to evaluate its condition during the nearest normal shut
down. Based on such investigations, it will be decided if superheater tubes are
still safe to be used under the working conditions or if it will be about to be
replaced with new tubes. In case of replacing tubes, header will also be replaced
with new one.
In order to decrease the possibility of such failure in future, the operation
conditions should be restrictly controlled to avoid overeating and then, to
increase the lifetime of superheater. Besides, periodic maintenance for checking
and evaluating of superheater condition using different non-destructive
inspection techniques then, carrying out necessary repair works is of
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Doc. X- 1639 - 08
considerable importance. During such periodic maintenance, removal of scale
from boiler tubes is recommended in order to avoid overheating of tubes. In this
regard, chemical or mechanical cleaning of tubes can be applied.

References
1. R. D. Port and H. M. Herro: The NALCO Guide to Boiler Failure Analysis,
McGraw-hil, Inc., USA, 1991.
2. A. El-Batahgy: "Catastrophic Failure of Waste Heat Boiler", Materials
Performance, February 1997.
3. V.J. Colangelo, F.A. Heiser: Analysis of Metallurgical Failures, 2nd. ed.,
New York, NY: Wiley, 1987.
4. R. D. Barer, B. F. Peters: Why Metals Fail, 6th ed., Gordon and Breach,
Science Publishers, New York, 1991.
5. A. El-Batahgy and W. Metwaly: Failure Analysis of Boiler Water WallTubes at a Power Generation Plant, The 31st Annual Convention of the
International Metallographic Society, 26 29 July 1998, Ottawa, Canada
6. Metals Handbook, Ninth Edition, Vol.11, Failure Analysis and Prevention,
ASM 1996.

Doc. X- 1639 - 08

Table 1 Chemical analysis of ruptured header and tube' materials, together

with the specified range for DIN 15Mo3 steel (wt%).
Element

Si

Material
ruptured header

0.200

0.223

ruptured tube

0.200

0.242 0.693

DIN 15Mo3 steel 0.12~

0.20

Mn

Mo

Fe

0.017

0.316

Bal.

0.010

0.019

0.280

Bal.

0.10~ 0.40~ 0.035

0.35
0.80 max.

0.035
max.

0.25~
0.35

Bal.

0.612 0.001

Table 2. Results of hardness measurements of ruptured header.

HV (l0kgf)
Zone
Outer surface
Ruptured zone

155

Mid-wall
thickness
163

Non-ruptured
zone

137

135

Inner surface

139

162

Table 3. Results of hardness measurements of superheater ruptured tube.

HV (l0kgf)
Zone
Outer surface
Ruptured zone

147

Mid-wall
thickness
151

Non-ruptured
zone

143

140

10

Inner surface

146

160

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Fig. 1. General and enlarged views of both ruptured and non-ruptured

samples of failed header. Note through-thickness cracking of
header' rupture zone

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Fig. 2. As-polished stereoscopic (a) and etched optical photographs (b, c, d)

of a cross section taken at front of header' ruptured zone showing
multiple cracks initiated sites close to outer surface and propagated
through grain boundaries voids.

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Fig. 3 Optical micrographs with different magnifications of a cross

section taken from header' ruptured zone showing partial
decomposition of pearlite into ferrite and spheroidal carbides
with voids.

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Fig. 4 Optical micrographs with different magnifications of a cross

section taken from header' non-ruptured zone showing partial
decomposition of pearlite into ferrite and spheroidal carbides
with voids

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Fig. 5 Scanning electron micrographs of a cross section taken from

header' ruptured zone showing decomposition of pearlite into
ferrite and spheroidal carbide particles in addition to voids

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Fig. 6 Scanning electron micrographs of header' fracture surface

showing large amount of voids, grain boundary cracking
and brittle fracture mode.

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Fig. 7 General view of ruptured tube before (a) and after (b, c, d) removing it
out of superheater showing bulging with fish-mouth shape rupture and
scale layer on both inner and outer surfaces of fracture zone.

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Fig. 8. Stereoscopic photographs of outer surface of fracture zone

showing exfoliation and cracking of thick scale layer
formed on outer surface.

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Fig. 9. Stereoscopic photographs of (a, b, c) inner surface of fracture

zone showing exfoliation and cracking of thick scale layer
formed on inner surface, and (d) fracture surface showing
thick-wall rupture or brittle fracture appearance.

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Fig. 10 Results of X-ray diffraction (XRD) analysis of scale layer

formed on superheater' tube surface. Note that magnetite
(Fe304) is the main component of this scale layer.

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Fig. 11 Optical micrographs of a cross section taken from rupture zone of

superheater tube showing complete decomposition of pearlite into
ferrite and spheroidal carbides with voids through tube thickness.

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Fig. 12 Optical micrographs of a cross section taken from non-rupture zone

of superheater tube showing complete decomposition of pearlite into
ferrite and spheroidal carbides with voids through tube thickness.

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Fig. 13 Scanning electron micrographs of a cross section taken from tube

rupture zone showing complete decomposition of pearlite into
ferrite and spheroidal carbide particles in addition to voids
and grains separation.

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Fig. 14 Scanning electron micrographs of tube rupture surface showing

large amount of voids, grains separation and the brittle fracture mode.

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