NACE Paper No.

MECCOCT18-12432

Sigma Phase Embrittlement in FCC Regenerator Secondary Cyclone

Mohammed Al Muaisub Suleiman Yero

Consulting Services Department Consulting Services Department
Saudi Aramco, Dhahran 31311 Saudi Aramco, Dhahran 31311
Saudi Arabia Saudi Arabia

ABSTRACT

This paper discusses a metallurgical failure analysis on broken parts of the FCC regenerator
secondary cyclone outlet gas tube in an aging refinery. The tube material is 304H SS, which
failed after (17) years of continuous operation. The cyclone service is flue gas and catalyst with
an operating temperature of 760 oC. The visual examination showed that the broken pieces
experienced thinning and a visible carburized layer. Moreover, upon conducting multiple
microhardness testing on the cross section of the sample, the hardness values were found to be
between 410 – 640 HV, more than twice the nominal value of the specified material. Also, after
preparing the sample for metallographic examination and selecting the proper etching, the
optical microscope showed severe sigma phase microstructure. Additionally, to further ensure
the presence of sigma phase, the sample was examined by the scanning electron microscopy
(SEM) technique using energy dispersive spectroscopy (EDS). The EDS analysis confirmed the
presence of the sigma phase in the microstructure. Therefore, based on the conducted tests, it
was found that the tube was severely sigmatized due to long-time exposure to high temperature.
Apparently, after a sudden decrease in the operating temperature under 260 0C during
shutdown, the sigmatized material exhibited lack of toughness, which then resulted in cracking
the embrittled parts.

Key words: Sigma Phase, Embrittlement, Carburization, Hardness Test, Failure Analysis, Damage
Mechanism, FFC, Regenerator, Cyclones
 INTRODUCTION

The Fluid Catalytic Cracking (FCC) is one of the critical conversion processes that is used in the
refineries. The FCC unit function is to convert the heavy hydrocarbon fractions of the crude oil
into gasoline and other products. It is critical to mention that about 50% of the refinery heavy
petroleum is processed through the FCC cyclones. The regenerator cyclones are used to
separate the catalyst from the flue gas created when the carbon or coke is burned with air from
the FCC catalyst. These regenerator cyclones are originally designed to sustain an abrasive
environment with a temperature reaching 780 oC. [1]

One of the common damage mechanisms that are experienced in FCC regenerator cyclones is
the sigma phase embrittlement. Sigma phase embrittlement is the formation of a metallurgical
phase, known as the sigma phase, which can result in a loss of fracture toughness in some
stainless steels as a result of high temperature exposure. The 300 series and 400 series of
austenitic, ferritic, martensitic, and duplex stainless steels (SS), are susceptible to this damage
mechanism, when the material is exposed to temperatures in the range of 1000 to 1750°F (538
to 954oC). [2]

In this paper, a detailed metallurgical investigation was conducted on broken parts of the FCC
regenerator secondary cyclone outlet gas tube in an aging refinery. The tube material is 304H
SS and it failed after (17) years of operation. The cyclone service environment is flue gas and
catalyst with an operating temperature of 760 oC.

LABORATORY TESTING

To properly investigate this failure, the broken pieces were visually examined and multiple
microhardness tests were conducted across the thickness of the broken pieces, to determine
their variation at the surface of the failed piece after exposure to high temperature. Moreover, a
representative sample was prepared for metallographic examination, and the proper etchant
was selected to reveal the sigma phase under the optical microscope. Finally, the sample was
examined by the scanning electron microscopy (SEM), and analyzed using energy dispersive
spectroscopy (EDS), to examine for the presence of the intermetallic compound in the
microstructure.
 RESULTS AND DISCUSSION

As mentioned in the introduction, the cyclone service environment is flue gas and catalyst, with
an operating temperature and pressure of 760oC and 43 psi, respectively.

The metallographic testing revealed the presence of the sigma phase in the microstructure
(Figures 1-4). The metallurgical and mechanical tests showed that the failure occurred due to
sigma phase embrittlement. It is known that sigma phase formation is a natural aging process
that occurs in 304H SS and other similar austenitic stainless steels, when exposed to high
temperature service between 538 oC to 927 oC for extended periods of time. Moreover, upon
cooling to temperatures under 260 oC during shutdown, the severely sigmatized material will
exhibit lack of toughness, thus making it susceptible to brittle fracture under excessive stresses.

Due to the sigma phase embrittlement, minor impact loading predominantly results in cracking;
leading to failure. Therefore, it is advisable to avoid excessive stresses during start-up,
shutdown, or maintenance activities.

Figure 1: Photographs shows broken pieces from the cyclone outlet gas tube in as-received
condition.
Figure 2: Close-up photograph shows a prepared cut sample from the broken piece. Note the thick
carburization layer.
Figure 3: Photomicrographs in as-etched condition show the sigma phase formation in the
microstructure.
 Figure 4: SEM micrograph shows the microstructure and a spot analysis in as-etched condition.

Figure 5: Photomicrograph in as polished condition. Note the embedded table illustrating the high
micro-hardness values at different layers.
 CONCLUSIONS

In conclusion, based on the metallurgical analysis and the microhardness test results, the failure
of the FCC regenerator secondary cyclone outlet gas tube is attributed to sigma phase
embrittlement. The optical microscope photographs showed the presence of sigma phase in the
etched sample. Moreover, the SEM/EDS analysis confirmed the presence of the sigma phase
in the microstructure.

REFERENCES

1. CECO Environmental, “FCC Cyclones – Regenerator,” https://www.cecoenviro.com/fcc-

cyclones-regenerator-emtrol-buell, 2018.
2. API RP 571 (Second Edition), “Damage Mechanisms Affecting Fixed Equipment in the
Refining Industry,” American Petroleum Institute (API), 2011.
3. Jorge Hau and Antonio Seijas, “Sigma Phase Embrittlement of Stainless Steel in FCC
Service,” NACE Corrosion Conference 2006, paper no. 6578, (Houston, TX: NACE, 2006).
4. A. M. Babakr, A. Al-Ahmari, K. Al-Jumayiah, and F. Habiby, “Sigma Phase Formation and
Embrittlement of Cast Iron-Chromium-Nickel (Fe-Cr-Ni) Alloys,” Journal of Minerals & Materials
Characterization & Engineering, Vol. 7, No.2, pp 127-145, 2008.