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Engineering Failure Analysis 59 (2016) 292303

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Engineering Failure Analysis


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Failure analysis and metallurgical transitions in SS 304L air pipe


caused by local overheating
D. Luder a,, T. Hundhausen b, E. Kaminsky a, Y. Shor a, N. Iddan a, S. Ariely a, M. Yalin a
a
b

Materials Lab, Israel Electric Corporation, Nativ Haor 1, Haifa 31000, Israel
Department of Materials Science, Technical University Darmstadt, Karolinenplatz 5, 64289 Darmstadt, Germany

a r t i c l e

i n f o

Article history:
Received 15 July 2015
Received in revised form 15 October 2015
Accepted 19 October 2015
Available online 19 October 2015
Keywords:
Failure analysis
Austenitic stainless steel
Creep
Overheating
Power-plant failures
Grain growth

a b s t r a c t
AISI 304 type stainless steels are widely used for structural parts in power stations due to their
excellent resistance to creep and corrosion at elevated temperatures. In an incident at one of
IEC's (Israel Electric Corporation) power stations, an air pipe made of AISI 304L Stainless
Steel which was part of a gas conditioning system conducting hot air for mixing with natural
gas, failed and cracked at two points. Failure analysis included stereo imaging, optical metallography, SEM/EDS/EBSD and magnetic tests. It was revealed that one crack occurred due to hightemperature overload and the other due to creep, showing grain coarsening and secondary
phase formations respectively to an extent that is entirely atypical under standard working
conditions. A follow-up investigation was conducted in order to gain further insight into the
processes and conditions that led to the two crack failures in the pipe. Thermal treatments
of intact specimens from an undamaged pipe area were conducted at different temperatures
and times. Pipe specimens subject to heat treatments of 650 C resembled material near the
creep fracture in the eld pipe. Pipe specimens subject to heat treatments of 1000 C and
1150 C resembled material near the high-temperature overload failure. The thermal treatment
was followed by microstructural, mechanical, compositional and phase analyses.
2015 Elsevier Ltd. All rights reserved.

1. Introduction
Stainless steels are common and widespread engineering alloys applied in many branches of industry such as food, petrochemicals and electric power industries [15]. In particular, austenitic stainless steels are commonly applied due to their excellent combination of mechanical properties and resistance to corrosion [6,7]. This steel class typically has chromium content between 18
and 20 wt.%, nickel content between 8 and 10.5 wt.%, and carbon content lower than 0.08 wt.%, as well as small percentages of
silicon, nitrogen and manganese [2]. High chromium content causes the formation of a dense passivation layer, enabling corrosion
resistance at room temperature and elevated temperatures. Nickel and manganese are added in order to stabilize the austenitic
phase for its mechanical properties, namely high-temperature ductility and creep resistance [2]. Carbon content is kept low to
avoid the formation of chromium carbides which lead to embrittlement and sensitization [2,8]. The addition of silicon also
leads to better corrosion resistance, especially at elevated temperatures. The combination of silicon and chromium provide superior corrosion resistance without high susceptibility to creep. AISI 304L steel has a reduced carbon content of 0.03 wt.% or lower
[8] which limits the precipitation of carbides, making it suitable for welding and for use in power plant applications, where gases
and air at high temperatures need to be transported to and from functional parts such as boilers and turbines [9]. One important

Corresponding author.
E-mail address: daniel.loder@iec.co.il (D. Luder).

http://dx.doi.org/10.1016/j.engfailanal.2015.10.014
1350-6307/ 2015 Elsevier Ltd. All rights reserved.

D. Luder et al. / Engineering Failure Analysis 59 (2016) 292303

293

application is its use in pipes that can sustain temperatures of up to 600 C for more than 10.000 h, making long-term creep and
corrosion resistance of prime importance [9].
In one of IEC's power plants red with natural gas, a pipe made of the above material failed and cracked at two different points
at the bottom of the pipe as seen in Fig. 1. The pipe is used for conducting hot air in a natural gas conditioning system (Gas conditioning skid) with the normal working parameters: service temperature: 350420 C, pressure: 35 MPa, wall thickness:
6.23 mm, OD: 114.4 mm (service period: 43,000 h). The two cracks exhibited distinctly different characteristics, leading to the
presumption that the two cracks occurred due to completely different mechanisms despite their close proximity on the pipe. Failure analysis was conducted by employing stereo imaging, optical metallography, SEM/EDS/EBSD and magnetic tests. Subsequently,
lab experiments were conducted in order to reconstruct the conditions under which the two cracks have been formed; an undamaged area of the pipe was cut and sectioned, and various heat treatment experiments were conducted on prepared specimens.
The analysis of the specimens and their comparison to the results of the prior crack failure analysis assisted in identifying the conditions and processes that led to the crack failures in the pipe.
2. Experimental methods
Camera images were taken with a DSLR camera. Stereoscopic images were taken with a stereoscope equipped with a digital
camera. Optical emission spectroscopy (OES) measurements were conducted using an ARC-MET 930 spectrometer.HR-SEM microscopy, EDS and EBSD analysis were performed with a Supra-40 microscope equipped with an XPlash EDS detector and a
NordlysNano EBSD detector. Specimens for optical metallography were prepared according to the ASTM A262-02a standard
and were observed in an optical microscope equipped with a digital camera.
Specimens for lab experiments were prepared by cutting an undamaged pipe area (Fig. 1) into pieces of 15 40 6.5 mm.
The specimens were subject to thermal treatments at varying temperatures and time intervals in a gravity convection furnace.
Magnetism tests were conducted with a conventional magnet. Grain size analysis was conducted according to the ASTM E112-96
standard. Hardness tests were conducted with a Wilson/Rockwell hardness tester (series 500) and Rockwell-B indenter according
to the ASTM E18-05 standard.
3. Failure analysis
3.1. Visual inspection
The pipe as found in the power station after failure, and the sectioned pipe part are presented in Fig. 1. The pipe is located at
the bottom part of the skid system.

Fig. 1. Air pipe (a) as found in the power station after failure (b) as observed after sectioning, sectioned pipe length: 80 cm.

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Fig. 2. (a) Crack 1 as marked in Fig. 1b, with sharp thin edges. (b) Crack 2 as marked in Fig. 1b, with rough and relatively thick edges.

The pipe had cracked at two locations at the bottom, and a deformed area devoid of cracks was observed between crack 2 and
an undamaged section with unaltered dimensions (Fig. 1b).Crack 1 exhibited sharp edges and severe tube wall thinning, often
observed in cases of high-temperature overload (crack 1. Figs. 1b and 2a).Crack 2 exhibited rough thick edges and relatively moderate tube wall thinning, often observed in cracks caused by creep failure (crack 2. Figs. 1b and 2b) [10].
The pipe circumference and wall thickness around the cracked areas, and an undamaged reference location (marked in Fig. 1b)
were measured and are presented in Table 1. It can be noticed that the circumferences around the cracked locations are much
longer than the undamaged area. Moreover, the pipe circumference around crack 1 was longer by 10 mm than the one around
crack 2. When diameters were measured at different angles around the circumferences of both cracks, the diameter along the
axis including the cracks was the longest. These measurements are complimentary to those of wall thickness which are much
thinner in the circumference of the cracked area compared to the undamaged area (additionally, wall thickness is slightly thinner
around crack 1 than around crack 2). These ndings indicate that, as expected, the pipe had undergone sever plastic deformation
in the lead-up to both crack formations. The larger circumference, thinner wall thickness and more severe plastic deformation of
crack 1 compared to crack 2 leads to the conclusion that higher temperatures existed in this location, also supporting the notion
that the failure type of crack 1 is closer in nature to high-temperature overload than the other crack [10].
At the bottom of the pipe, a relatively large quantity of ash was found. This indicates that an organic matter may have undergone combustion at this location,
3.2. Stereoscopic imaging
Observations of crack 1's surface using a stereoscope (Fig. 3a) show that the wall thickness had decreased substantially at the
edge (b 1 mm) in similarity to the edges of ductile cupcone tensile fractures. This nding, and the presence of equiaxed dimples
and severe deformation in the direction of stress (circumferential) further suggests that the crack developed as a result of overload at high temperatures [11,12].
The surface of crack 2 (Fig. 3b) is much wider and rough with deep and large voids, at this stage raising the suspicion that
these are actually coalesced creep voids formed at the third and nal stage of creep failure. Additionally, it could be seen that
the surface contained scale and multiple brittle appearing ssures that are consistent with creep fracture surfaces [11,12].
3.3. Chemical analysis
The chemical composition of the pipe material was determined by optical emission spectroscopy (OES) in order to accurately
identify the pipe material. The results are presented in Table 2. The pipe material was conrmed to be 304L. Chemical analysis of
ash found near the cracks was also performed using EDS with results presented in Table 3. High oxygen content suggests that the
ash is a result of organic fuel combustion and extreme heat near the pipe surface, resulting in severe oxidation of the steel. The
origin of remnants such as Al and Ca is suggested to be from impurities originating from primary plant processes.
3.4. Optical metallography
OM images of material near the tip of crack 1 are presented in Fig. 4. By comparing Fig. 4ad it is noticeable that the grains
closer to the crack tip are about one order larger than grains located in the reference area far from the tip, evidence of grain
Table 1
Wall thickness and diameter of rings cut from the sectioned air pipe at different locations.
Pipe ring

Average wall thickness [mm]

Average pipe ring diameter OD [mm]

Pipe ring including crack 1


Pipe ring including crack 2
Pipe ring cut from undamaged pipe section (reference, nominal dimensions)

4.8
5
6.23

157
147
114.4

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Fig. 3. (a) Surface of crack 1 as marked in Fig. 2a, with sharp thin edges. (b) Surface of crack 2 as marked in Fig. 2b, with rough and relatively wide edges.

growth and recrystallization near the crack. At about 3 mm away from the tip, not only are the grains much larger than the grains
far from the crack, they also deformed in the direction of the crack. Substantial grain growth, recrystallization and directional deformation near the crack are evidence of exposure to high temperatures and stress. At the tip itself (Fig. 4a) strain bands are clearly prominent, showing that the material underwent substantial plastic deformation before the failure had occurred. An additional
aspect is the presence of strain bands at the reference area far from the crack (Fig. 4d), their disappearance at 36 mm away from
the crack (Fig. 4bc) and reappearance at the crack tip itself. This can be explained due to residual strains left over from the
manufacturing process far from the crack, exposure to intense heat near the tip causing annealing, and the reappearance of strain
bands at the tip due to high deformation. Evidence of high temperatures and stresses near the crack tip further support the notion
that a high-temperature overload failure had occurred at this location.
OM images of crack 2 are presented in Fig. 5. The most prominent feature is the presence of voids near the crack (Fig. 5ac),
absent from the reference area far from the crack (Fig. 5d). Moreover, the voids grow in diameter by one order of magnitude as
they approach the tip (from ~50 m in Fig. 5c, to ~120 m in Fig. 5a). A second prominent feature is the presence of secondary
phases at the grain boundaries. The voids correspond to creep with wedge type cavities [10], characterized by nucleation and
growth at triple points. On the surface of the crack tip (Fig. 5a) there is a thick scale layer, also indicative of high temperature
conditions leading to creep.
3.5. Magnetism
A magnet was attached to the three pipe rings mentioned in Table 1. The ring containing crack 1 was Ferro-magnetic to a
small extent. The ring including crack 2 (with suspected creep crack) was shown to be strongly Ferro-magnetic, especially near
the crack tip. Contrarily, the reference ring from the undamaged section was not Ferro-magnetic.
The Ferro-magnetism appearing near and around crack 2 (and to a lesser extent with crack 1) is indicative of the precipitation of a
Ferro-magnetic phase, such as the phase at the grain boundary as seen in Fig. 5, while bearing in mind that the regular austenitic bulk
phase is non-magnetic. In light of the low carbon content in the current material (lowering the probability of carbide formation) there
is a possibility that this phase is -ferrite [13], a possibility that warrants investigation in light of its magnetic properties.
3.6. SEM imaging
The surfaces of crack 1 and crack 2 are presented in Fig. 6. In Fig. 6a (crack 1) the surface is characterized by very low wall
thickness at the tip (~120 m compared to 6.23 mm at the undamaged section) and non-directional dimples, typical of ductile
fractures and high-temperature overload in particular [1012], as suggested in previous paragraphs.
Table 2
Chemical composition of pipe material (S-OES).
Element

Content [wt.%]

304L ASTM-A312

Cr
Ni
Mn
Si
C
Co
Cu
Nb
Mo

18.34
8.79
1.81
0.3
0.032
0.48
0.21
0.12
0.11

1820
811
Max. 2.00
Max. 1.00
Max. 0.035

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D. Luder et al. / Engineering Failure Analysis 59 (2016) 292303


Table 3
Chemical composition of ash from the pipe (EDS).
Element

Content [wt.%]

Fe
O
Mn
Ni
Cr
Al
Si
Ca

68.7
24.5
2.2
2.2
2
0.2
0.1
0.1

In Fig. 6b (surface of crack 2) large voids can be observed, corresponding to the creep voids observed in Fig. 5. The wall thickness at the tip is much higher than in crack 1 (2 mm compared to 120 m), an additional feature common to creep failures which
highlights the fact that both cracks are completely different in nature [1012].
4. Lab experiments
A follow-up investigation has been conducted in order to gain further insight into the processes that occurred at the crack locations and to partially reconstruct the conditions under which they had formed. Thermal treatments of specimens from the undamaged pipe section (Fig. 1) were conducted at different temperatures and time intervals followed by microstructural, compositional,
mechanical, and phase analysis. The thermal treatments were conducted according to Table 4.
4.1. Microstructure analysis
4.1.1. Optical metallography
OM images of specimens, sectioned from the undamaged pipe area, after thermal treatments at 650 C are presented in Fig. 7:
In Fig. 7a (reference specimen) the average grain diameter is 0.019 0.003 mm. A substantial quantity of secondary phase
can be noticed at the grain boundaries at a preferential orientation. It is suggested that this preferential orientation is congruent

Fig. 4. OM images of area near the tip of crack 1: (a) crack tip (b) 3 mm from crack tip (c) 6 mm from crack tip (d) reference area far from crack tips.

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Fig. 5. OM images of area near the tip of crack 2: (a) crack tip; (b) 3 mm from the crack tip; (c) 6 mm from crack tip; (d) reference point far from crack tip.

with the directional strain bands left over from the manufacturing process. As the thermal treatment proceeds in Fig. 7b and c it
can be noticed that the average grain size hardly changes. However, a secondary phase that had existed in the reference specimen
had continued to precipitate at the grain boundaries and also the bulk, eventually covering almost the entire grain boundary
surface.
OM images of specimens (originally from the undamaged pipe area) after thermal treatments at 1000 C are presented in
Fig. 8:
In the above samples, not only was there no observation of secondary phase precipitation, but the secondary phase that had
existed in the beginning had disappeared, leading to the notion that the chemical constituents of this phase were at a high
enough temperature to have full solubility in the bulk steel phase. Instead, twin grain boundary, low-angle grain boundary formation, and increasing grain coarsening with time could be observed. At these temperatures, the thermodynamic equilibrium favors
the presence of large grains over the precipitation of secondary phases [14,15].
OM images of specimens (originally from the undamaged pipe area) after thermal treatments at 1150 C are presented in Fig. 9:

Fig. 6. SEM images of (a) surface of crack 1 and (b) surface of crack 2.

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Table 4
Treatment times (hours) of sectioned specimens taken from the intact undamaged pipe
area.
650 C

1000 C

1150 C

4
8
24
168

0.5
1
2
4

0.5
1
2
4

As in the previous thermal treatment, at 1150 C there was no secondary phase precipitation. The grain coarsening, low angle
boundary and twin grain boundary formation were quicker to appear and much more pronounced than at 1000 C.
4.1.2. Grain size analysis
Grain size analysis by the use of the intercept method mentioned in ASTM E 112-96 was conducted on all samples. The analysis included statistical error estimation by means of calculating the standard deviation.
Fig. 10 shows the average grain diameters of all thermal treatments, and for every time interval (as presented in Table 4 and
illustrated in Figs. 79), with the value of the reference sample at 0 h.
From the grain growth comparison above it can be observed that the rate of grain coarsening increases with temperature.
Moreover, an increase in temperature has a much larger effect on grain growth at short time intervals than an increase in treatment
time. These ndings conrm the ndings of the previous paragraph where it was seen that at the 10001150 C range there is a thermodynamic preference for grain growth, in contrast to a 650 C environment characterized by the lack of detectable change in grain
size.
4.1.3. Hardness tests
In order to correlate grain growth and mechanical properties while shedding light on the materials properties at the time of
failure, hardness tests were conducted on all samples using the Rockwell B method. Results are displayed in Fig. 11:
At 650 C, the hardness changes only slightly, in parallel to the stability of grain size as discussed in earlier paragraphs. Minor
uctuations can be associated with the precipitation of secondary phases, with characteristics which are to be discussed.
At 1000 C and 1150 C, a general softening trend is clearly observed, corresponding to the increase in grain size mentioned
before. Due to faster grain growth observed for the material at 1150 C, it is not surprising that softening had occurred more rapidly (and to lower values) than at 1000 C.
4.1.4. Comparison between experimental images and failure analysis
A comparison between the specimen images taken after the heat treatments and the images taken around the cracks are presented in Fig. 12.
When comparing the areas near the cracks and the specimens taken from the undamaged area, a similarity between the microstructures can be observed. The specimen thermally treated at 1150 C for 4 h (Fig. 12a) had an average grain size that was similar
to the area 6 mm from crack 1(Fig. 12b) within the error range (Fig. 10).
The specimen thermally treated at 650 C after 168 h (Fig. 12c) exhibits secondary phase precipitation over virtually the entire
grain boundary area (and also at the bulk to a lesser extent), in a similar way observed 6 mm away from crack 2 (Fig. 12d). The
grain diameter of the experimental specimen was relatively close to the average diameter near the crack, being 1020% smaller.
The distorted grains in Fig. 12b,d and the presence of creep voids in Fig. 12d (in contrast to their absence in Fig. 12a,c) is
explained by the continuous pressure bored by the pipe in working conditions. It can nally be deduced that crack 1 and 2
were subject to completely different temperature conditions; crack 1 was exposed to temperatures within the range of (or approximately near to) 10001150 C before failing due to high-temperature overload, and crack 2 was exposed to temperatures

Fig. 7. OM images of specimens after thermal treatments at 650 C after (a) 0 h, (b) 4 h and (c) 168 h.

D. Luder et al. / Engineering Failure Analysis 59 (2016) 292303

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Fig. 8. OM images of specimens after thermal treatments at 1000 C for (a) 0 h, (b) 0.5 h and (c) 4 h.

within a range around 650 (with the exact range being unknown) before failing due to creep. Previously analyzed ash remnants
suggested to be a result of condensed gas combustion, increase the probability of high temperature regimens mentioned above.
The softening phenomena measured for the experimental specimens treated at 10001150 C (Fig. 11) is complementary to the
high-temperature overload failure seen for crack 1, such failures are known to be accompanied by heat, annealing and softening
which substantially lowers the material's yield and tensile strengths.
4.2. Secondary phase analysis
The secondary phase prominently observed around crack 2 and the specimens treated at 650 C is of great interest and can shed
further light on the processes that had occurred in the pipe. EDS map imaging of a pipe specimen taken from the undamaged section
(treated at 650 C for 168 h) is presented in Fig. 13, and the chemical contents of the secondary phase and the bulk near the grain
boundary are presented in Table 5:

Fig. 9. OM images of specimens after thermal treatments at 1150 C for (a) 0 h, (b) 0.5 h and (c) 4 h.

Fig. 10. Average grain diameters vs. time for thermal heat treatments performed at 650 C, 1000 C and 1150 C.

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Fig. 11. Average hardness values (HRB) vs. time for thermal heat treatments at 650 C, 1000 C and 1150 C.

The secondary phase has a much higher Cr content and has lower Fe, Ni and Mn content compared to the bulk. When comparing these ndings to the literature, it is strongly suggested that this secondary phase is -Ferrite, a Cr-rich Ferro-magnetic
phase [13]. In addition to the chemical content, earlier it was found that the area around crack 2 was Ferro-magnetic; in the
case of the examined specimen magnetism was also detected. Due to the low carbon content (Table 1), it is highly improbable
that the phase is a carbide.
In order to further verify the above phase, EBSD analysis was conducted on the secondary phase and the surrounding bulk. The
SEM (back scattered electron contrast) image, diffraction pattern(Kikuchi lines) and corresponding computer ts are presented in
Fig. 14:
The diffraction pattern presented in Fig. 14B and the corresponding t in Fig. 14C match the austenitic phase, as expected of
bulk 304L steel. The pattern in Fig. 14D and the corresponding t in Fig. 14E match -Ferrite.

Fig. 12. Comparison between (a) an intact undamaged pipe specimen after thermal treatment of 1150 C after 4 h and (b) an area 6 mm from crack 1. Comparison
between (c) an undamaged pipe specimen after thermal treatment of 650 C after 168 h, and (d) an area at 6 mm from crack 2.

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Fig. 13. Secondary phase observed in specimen taken from undamaged pipe section, treated at 650 C for 168 h: (a) SEM image; (b) Fe concentration; (c) Cr
concentration.

It can be concluded that the precipitation of -ferrite as the secondary phase has been conrmed by EBSD phase analysis, as
suggested after previous magnetic tests and EDS analysis.
5. Conclusions
By applying visual inspection, stereographic imaging, optical metallography and SEM imaging it was established that the nding designated as crack 1 failed due to high-temperature overload and crack 2 failed due to creep. Chemical analysis of the ash
(found in the crack's vicinity) via EDS revealed the prospect that the cracks had developed in parallel to organic fuel combustion
near the cracks. Magnetic tests revealed that the ring containing crack 2 (and to a lesser extent around crack 1) was Ferromagnetic, in contrast to the undamaged pipe area and 304L stainless steel in general. This led to the conclusion that a Ferromagnetic phase had precipitated in parallel with the cracks development, especially in crack 2.
After conducting the follow-up investigation which included the application of optical metallography and comparison of the
results to the images found near the cracks, it was strongly suggested that a temperature regimen between 1000 and 1150 C
had existed around crack 1 during the high-temperature overload crack formation, and that a temperature regimen within a
range around 650 C (with the exact range being unknown) existed around crack 2 during creep progression.
Grain growth and softening phenomena measured for specimens treated at 10001150 C (and the lack of such phenomena
for species treated at 650 C) are complementary to the material conditions expected prior to the high-temperature overload failure seen for crack 1 and creep failure seen for crack 2.
From calculations conducted in the lab taking account of modied mechanical properties at the high temperatures and circumferential stress calculations, it is estimated that a peak pressure of 3545 MPa existed in the pipe (in contrast to 35 MPa in
normal working conditions) prior to the bursts, indicating creep duration of less than 100 h at 650 C [16]. The possibility of
high-temperature conditions and creep development during longer periods such as the whole service period (43,000 h, 650 C)
was ruled out due to the requirement of having a pressure of 910 MPa [16] in the pipe for extended periods at elevated temperatures, a situation which station operators had reported was not possible due to operational monitoring and periodical visual
inspections.
Finally, the magnetic secondary phase found mostly around crack 2 and the specimens treated at 650 C were investigated via
EDS mapping and EBSD analysis. Mapping revealed that the secondary phase was rich in chromium while EBSD revealed that the
phase was -Ferrite, ndings consistent with the magnetism detected around the corresponding area.
The above ndings later on led to an additional investigation regarding the possibility of a gas leak into the air pipe, and subsequent gas condensation and combustion. It was concluded by the lab and investigators in the company that condensate gas had
accumulated in the pipe due to a valve leak, and started to combust. It was highly probable that there were at least two ignition
points near crack 1 and 2 with varying intensities. The mentioned process caused two different high temperatures at the two
points and the high pressures mentioned previously.

Table 5
Elemental composition of bulk material and secondary phase (at the grain Boundary); specimen taken from undamaged pipe section, treated at 650 C for
168 h.
Element

Bulk content near grain boundary [wt.%]

Secondary phase at grain boundary [wt.%]

Fe
Cr
Ni
Mn
Mo

67.3
16.4
7.9
2
0.11

57
30.7
5.5
0.8
~0

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Fig. 14. (A) SEM (back scattered electron contrast) image of points subjected to EBSD, Bulk (continuous arrow) and secondary phase precipitate (dashed arrow).
(B) Diffraction pattern of Bulk. (C) Program t for bulk diffraction. (D) Diffraction pattern of secondary phase precipitate. (E) Program t for secondary phase
diffraction.

Acknowledgments
The authors would like to thank Mr. Gad Tsar (IEC) for assisting in operating various equipment and xing malfunctions
when needed, and Mr. David Zirkin for assisting in proofreading. The nancial assistance of the Vice president for Planning,
Development & Technology (Israel Electric Corporation) is acknowledged.

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Title
Failure analysis and metallurgical transitions in SS 304L air pipe caused by local overheating

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