Sigma phase (σ) is a brittle intermetallic compound that forms within the microstructure of stainless steels when exposed
to elevated temperatures (typically between 540°C
and 980°C) for extended periods. Its composition is primarily iron and chromium (Fe-Cr), but not in a simple ratio. The exact proportions can vary slightly depending on the
specific stainless steel and the formation temperature. it typically contains around 40-50% iron and 45-55% chromium. Other elements present in trace amounts within the
stainless steel,
286such as molybdenum, nickel, or silicon, might also API
be incorporated
RECOMMENDED into the sigma phase
PRACTICE 571 structure in small quantities. The complexity of the sigma phase arises
from its crystallographic structure. Unlike the face-centred cubic (FCC) structure of austenite or the body-centred cubic (BCC) structure of ferrite, common in stainless steels,
sigma adopts a tetragonal crystal lattice which has has unequal side lengths along different axes. The tetragonal structure of sigma phase is an inherently brittle.
The strong interatomic bonds within the σ phase, and unequal atomic packing limit its ability to deform or
3.56 Sigma Phase Embrittlement bend, restricts slip and dislocation movement. This intricate arrangement of atoms within the lattice makes
it lack the ductility and toughness characteristic of the surrounding stainless-steel matrix.
3.56.1 Description of Damage
Formation of a metallurgical phase known as sigma phase in some stainless steels when they are heated above
about 1000 °F (540 °C) can result in a loss of ductility and fracture toughness. The embrittlement can lead to
cracking failure. Many stainless steels and other iron-chromium alloys are susceptible to a grain boundary phenomenon known as
sigma-phase embrittlement. The major effects of this phenomenon are the loss of ductility, toughness, and corrosion
resistance, which results in the failure of the material.
3.56.2 Affected Materials
a) 300 series SS wrought metals, weld metal, and castings. Cast 300 series SS including the HK and HP alloys
are especially susceptible to sigma formation because of their high (10 % to 40 %) ferrite content.
b) 400 series SS and other ferritic and martensitic stainless steel with > 17 % Cr are also susceptible (e.g. Types
430 and 440).
The formation of the sigma phase on the material depends on the ferrite content of the material, that is;
higher the ferrite content the higher the formation will be. The sigma phase formation will be rapid in
c) Duplex stainless steels. ferritic stainless steel, moderate in duplex stainless steel, and slower in austenitic stainless steel.
3.56.3 Critical Factors
a) Alloy composition, temperature, and time at temperature are the critical factors.
In susceptible alloys, the primary factor that affects sigma phase formation is the time of exposure at
elevated temperature.
b) The metallurgical change is a precipitation of a hard, brittle intermetallic compound that can also render the
material more susceptible to intergranular corrosion. The precipitation rate and amount increases with
increasing chromium and molybdenum content.
c) Sigma phase forms in ferritic (Fe-Cr), martensitic (Fe-Cr), austenitic (Fe-Cr-Ni), and duplex stainless steels
when exposed to temperatures in the range of 1000 °F to 1700 °F (540 °C to 925 °C). Embrittlement can
result by holding within or cooling through the transformation temperature range.
d) Sigma forms most rapidly from the ferrite phase that exists in 300 series SS and duplex stainless steel weld
deposits. It also readily forms in duplex stainless steel base metals due to their nominally 50 % ferrite phase.
It can also form in 300 series SS base metal (austenite phase) but usually more slowly.
e) Some 300 series SS can exhibit about 10 % to 15 % sigma phase. Cast austenitic stainless steels, which
typically have a high ferrite content (up to 40 %), can develop considerably more sigma than wrought
austenitic stainless steels, and may have very poor high-temperature ductility.
f) Formation of sigma phase in austenitic stainless steel weld metals can occur in a few hours, as evidenced
by the tendency for sigma to form in austenitic stainless steel weld overlay subjected to a PWHT at 1275 °F
(690 °C) during the fabrication of heavy wall pressure vessels.
g) The tensile strength and yield strength of sigmatized stainless steels increases slightly compared with
solution annealed material. This increase in strength is accompanied by a reduction in ductility (measured by
percent elongation and reduction in area) and a slight increase in hardness.
h) Stainless steels with sigma can normally withstand operating stresses at operating temperatures but upon
cooling below about 500 °F (260 °C) may show a complete lack of fracture toughness as measured in a
Charpy impact test. Laboratory tests of embrittled weld metal have shown a complete lack of fracture
toughness below 1000 °F (540 °C).
Tests performed on sigmatized 300 series SS (304H) samples from FCC regenerator internals have
shown that even with 10 % sigma formation (a large amount), the Charpy impact toughness was still
39 ft-lb (53 J) at 1200 °F (650 °C).
Sigmatized Stainless Steel: has Sigma phase, a brittle compound, forms unintentionally at 1000–1700 °F in Cr- and Mo-rich alloys like welds.
Solution-Annealed Stainless Steel: Heated to 1850–2050 °F and quenched, it dissolves precipitates for a uniform, ductile austenite structure.
eld long enough to dissolve precipitates (like carbides or sigma phase) into the matrix, and then rapidly cooled (quenched) to "lock in" a uniform,
single-phase microstructure.
Key Difference: Sigmatized steel is stronger but brittle; solution-annealed is softer but tougher.
Purpose: Sigma occurs during service; solution annealing restores optimal properties.
DAMAGE MECHANISMS AFFECTING FIXED EQUIPMENT IN THE REFINING INDUSTRY 287
For the 10 % sigmatized specimen, the values ranged from 0 % ductility at room temperature to 100 %
at 1200 °F (649 °C). Thus, although the impact toughness is reduced at high temperature, the specimens
broke in a 100 % ductile fashion, indicating that the wrought material is still suitable at operating
temperatures. (See e.g. Figure 3-56-2.)
3.56.4 Affected Units or Equipment
a) Common examples include stainless steel cyclones, piping ductwork, and valves in high-temperature FCC
regenerator service.
b) 300 series SS weld overlays and tube-to-tubesheet attachment welds can be embrittled during PWHT of the
underlying Cr-Mo base metal.
c) Stainless steel heater tubes are susceptible and can be embrittled.
3.56.5 Appearance or Morphology of Damage
a) Sigma phase embrittlement is a metallurgical change that is not readily apparent, and can only be confirmed
through metallographic examination (Figure 3-56-3 to Figure 3-56-5) and impact testing (Table 3-56-1 and
Table 3-56-2 and Figure 3-56-1).
b) Damage due to sigma phase embrittlement appears in the form of cracking, particularly at welds or in areas
of high stress or high restraint.
c) Most cases of embrittlement are found in the form of cracking in both wrought and cast metals, including
welds, during turnarounds, or during start-up or shutdown when the material is below about 500 °F (260 °C)
and the effects of embrittlement are most pronounced.
3.56.6 Prevention/Mitigation
a) The best way to prevent sigma phase embrittlement is to use alloys that are resistant to sigma formation or
to avoid exposing the material to the embrittling temperature range.
b) Because of the lack of fracture ductility at room temperature, care should be taken to avoid application of
high stresses to sigmatized materials during a shutdown, as a brittle fracture could result.
c) 300 series SS can be de-sigmatized by solution annealing at 1950 °F (1065 °C) for 4 hr followed by a water
quench. However, this is not practical for most equipment.
d) Sigma phase in welds is typically minimized by controlling the ferrite content, i.e. by specifying the allowable
range of ferrite in the weld metal, e.g. in the range of 5 % to 9 % for Type 347 and somewhat less ferrite for
Type 304. Limiting the maximum ferrite content minimizes sigma formation during service or fabrication. The
minimum ferrite content is needed to minimize hot short cracking during welding.
e) For stainless steel weld overlayed Cr-Mo components, the fabrication plan and sequence should attempt to
minimize the exposure of the overlay to base metal PWHT temperatures wherever possible, particularly in
highly stressed locations.
3.56.7 Inspection and Monitoring
This damage mechanism is very difficult to find and is also time dependent. Thus, it may take a while to develop
in service. Online inspection is not applicable. Awareness of susceptible equipment can help direct inspection
planning.
a) Sigma phase formation and embrittlement can be detected by removing and lab testing a sample of the
suspect material. Metallographic examination and/or impact testing can be used, as applicable.
288 API RECOMMENDED PRACTICE 571
b) For duplex stainless steels, ECT has been reported to find sigma phase embrittlement, primarily due to the
change in microstructure. However, this is highly dependent upon the methodology employed as well as the
knowledge and experience of the equipment operator.
c) FMR can be used to verify the presence of sigma phase in severe cases but normally will only assess the
condition at the surface of the component, not the thru-wall extent of the damage.
FMR field metallographic replication
3.56.8 Related Mechanisms
885 °F (475 °C) embrittlement (3.1).
3.56.9 References
1. API Recommended Practice 581, Risk-Based Inspection Methodology, American Petroleum Institute,
Washington, DC.
2. High Temperature Corrosion in Refinery and Petrochemical Service, High Temperature Engineering Bulletin
HTB-2, INCO, New York, NY, 1960.
3. L. Garverick, Corrosion in the Petrochemical Industry, ASM International, 1994, pp. 29 and 129–136.
4. R. Viswanathan, Damage Mechanisms and Life Assessment of High-temperature Components, ASM
International, 1989.
5. Metals Handbook—Desk Edition, ASM International, Materials Park, OH.
6. J. Hau and A. Seijas, “Sigma Phase Embrittlement of Stainless Steel in FCC Service,” Paper No. 06578,
Corrosion/2006, NACE International, Houston, TX.
7. API Recommended Practice 577, Welding Inspection and Metallurgy, American Petroleum Institute,
Washington, DC.
8. C.N. McCowan T.A. Siewert, and D.L. Olson, Stainless Steel Weld Metal: Prediction of Ferrite Content, WRC
Bulletin 342, Welding Research Council, Shaker Heights, OH, 1989.
9. E.L. Creamer et al., “Embrittlement of Type 347 Stainless Steel Weldments by Sigma Phase,” Welding
Research Supplement, June 1969, pp. 239–244.
10. G. Psuj, T. Chady, and C.G. Camerini, “Eddy Current Transducer Dedicated for Sigma Phase Evaluation in
Duplex Stainless Steel,” Journal of Sensors, Vol. 2012, 2012.
11. K. Doughten, D. Bauer, M. Rakos, and P. Domenico, “Non-destructive Testing of Duplex Stainless Steel,”
Stainless Steel World Americas Conference and Expo, October 2012.
12. J. Hau, “Sigma Phase Embrittlement of Type 304H Stainless Steel After FCCU Service,” Paper No. 09140,
Corrosion/2017, NACE International, Houston, TX.
DAMAGE MECHANISMS AFFECTING FIXED EQUIPMENT IN THE REFINING INDUSTRY 289
Table 3-56-1—Data for Property Trends of Toughness vs Temperature
304 SS 321 SS 304 SS 304 SS 347 SS
Test 2 % Sigma 10 % Sigma 1 % Sigma 2 % Sigma 1 % Sigma
Temperature
% of % of % % of % % of % % of %
% Shear
Impact Impact Shear Impact Shear Impact Shear Impact Shear
70 °F (21 °C) 21 0 7 0 — — 21 10 30 90
500 °F (260 °C) 38 25 10 20 — — — — 100 100
900 °F (480 °C) 44 50 15 40 20 10 — — 100 100
1200 °F (650 °C) 63 100 21 60 71 90 77 90 100 100
NOTE 1 Percent of impact is a comparison to original impact strength of non-embrittled materials.
NOTE 2 The results for 304 SS in columns one and four are for different heats of material under different exposure conditions and are
intended to exemplify variability of embrittlement.
Table 3-56-2—Charpy V-notch (CVN) Impact Test Results,
Absorbed Energy in Joules (ft-lb) from Reference 6
Sigma Phase Temperature
Refinery Location Years of Service
Content (%) RT Service
A Base metal 17 4.0 85 (63) 145 (107)
A Weld metal 17 8.7 37 (27) 100 (74)
B Base metal 19 12.0 12 (9) 43 (32)
C Base metal 13 1.5 35 (26) 75 (55)
290 API RECOMMENDED PRACTICE 571
Figure 3-56-1—CVN impact test results as absorbed energy in ft-lb,
at room temperature and service temperature. (Reference 6)
(b)
Figure 3-56-2—Tensile tests from 304H stainless steel FCC flue gas line with
12 % sigma phase. The top bar (a) failed in a brittle manner at room temperature.
The bottom sample (b) was tested at the operating temperature and shows
significant ductility and elongation at 1320 °F (716 °C). (Reference 6)
SIGMA PHASE EMBRITTLEMENT
Description Appearance
Loss of fracture toughness in A metallurgical embrittlement
stainless steels after high- only confirmed by
temperature exposure metallographic and impact test
Inspection: Not detectable using visual examination (VT).
Metallurgical (replication) tests of the
microstructure.
Charpy impact testing of test specimens.
Critical factors: Affects stainless steel with high ferrite content
(300 and 400 series). Cast austenitic (300) grades
are most susceptible.
The brittle intergranular 'sigma phase' occurs at
temperatures 538-927°C (1000-1700CF).
FFP/Severity: The material becomes harder and more brittle.
FFP assessment is very difficult as the decrease
in ductility and increase in brittleness is variable
and unpredictable. Metallographic replicas are
open to different technical interpretations.
References: API 571 (4.2.6)
API RP 581 Risk Based Inspection
DAMAGE MECHANISMS AFFECTING FIXED EQUIPMENT IN THE REFINING INDUSTRY 291
Figure 3-56-3—Microstructure of FCC regenerator plenum chamber wall,
electrolytic etch in 33 % KOH, magnification 100X. Dark-etching particles
are sigma phase; estimated amount is 6.0 %. (Reference 6)
Figure 3-56-4—Dark-etching particles are sigma phase that are concentrated near the outside surface
of FCC regenerator plenum chamber, electrolytic etch in 33 % KOH, magnification 100X. (Reference 6)
292 API RECOMMENDED PRACTICE 571
Figure 3-56-5—304H stainless steel with 14 years operation at a nominal temperature of
1320 °F (716 °C) after (a) etching in Vilella’s reagent, magnification 100X, and (b) electrolytic
etching in KOH, magnification 200X. The estimated amount of sigma phase was 5.0 %. (Reference 6)
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Sigma Phase Embrittlement: A Deep Dive into Stainless Steel’s Brittle
Phenomenon
PhD. MSc. MIcorr. NACE Senior Corrosion Technologist. Senior Corrosion
Consultant at Add-value consultancy
March 11, 2024
Sigma phase embrittlement (SPE) is a detrimental high-temperature damage
mechanism (DM) affecting various stainless-steel alloys. This article explores the
metallurgical and chemical reasons behind SPE susceptibility in 300, 400, and duplex
stainless steels, while highlighting the superior resistance of high-nickel alloys. The
influence of ferrite content and its transformation into sigma phase will be examined
in detail.
What is Sigma Phase?
Sigma phase (σ) is a brittle intermetallic compound that forms within the
microstructure of stainless steels when exposed to elevated temperatures (typically
between 540°C and 980°C) for extended periods. Its composition is primarily iron
and chromium (Fe-Cr), but not in a simple ratio. The exact proportions can vary
slightly depending on the specific stainless steel and the formation temperature.
However, it typically contains around 40-50% iron and 45-55% chromium. Other
elements present in trace amounts within the stainless steel, such as molybdenum,
nickel, or silicon, might also be incorporated into the sigma phase structure in small
quantities.
Why is Sigma Phase Complex and Brittle?
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The complexity of the sigma phase arises from its crystallographic structure. Unlike
the face-centred cubic (FCC) structure of austenite or the body-centred cubic (BCC)
structure of ferrite, common in stainless steels, sigma adopts a tetragonal crystal
lattice. This tetragonal structure means the unit cell, the fundamental building block
of the crystal, has unequal side lengths along different axes. The tetragonal structure
of sigma phase is an inherently brittle. The strong interatomic bonds within the σ
phase, and unequal atomic packing limit its ability to deform or bend, restricts slip
and dislocation movement. This intricate arrangement of atoms within the lattice
makes it lack the ductility and toughness characteristic of the surrounding stainless-
steel matrix.
Susceptibility of Different Alloys
• 300 and 400 Series Stainless Steels:These austenitic and ferritic-austenitic
(duplex) alloys are particularly susceptible to sigma phase embrittlement due to a
critical balance between chromium and nickel at the atomic level. Chromium (Cr) is a
key player in σ phase formation. Its strong affinity for iron (Fe) readily forms Fe-Cr
rich bonds, acting as the building blocks for the sigma phase lattice. Nickel (Ni), on
the other hand, acts as a stabilizing element, hindering σ phase development. Unlike
chromium, nickel atoms have a different size and electronic configuration. When
incorporated into the crystal lattice, they disrupt the orderly arrangement of Fe-Cr
atoms preferred for σ phase formation. This disrupts the growth of the σ phase and
promotes a more stable austenitic structure with a random distribution of atoms,
including nickel, throughout the lattice.
• High-Nickel Alloys:Alloys with significantly higher nickel content, such as Alloy
625 or Alloy 800, exhibit superior resistance to SPE. High-nickel alloys boast superior
resistance to sigma phase embrittlement (SPE) due to a synergistic effect at the
atomic level. Here's a breakdown of the key factors:
1- Disruption of Fe-Cr bonds:As mentioned earlier, chromium (Cr) readily forms
strong bonds with iron (Fe), which are the building blocks for the sigma phase lattice.
Nickel (Ni), with its different size and electronic configuration, disrupts this "chemical
handshake" between Fe and Cr atoms. Nickel atoms essentially act like "spacers"
within the lattice, hindering the formation of the ordered Fe-Cr rich regions necessary
for sigma phase nucleation.
2- Promotion of a stable austenitic structure:Nickel's presence promotes a
more stable austenitic microstructure. In austenite, the atoms (including nickel) are
randomly distributed throughout the face-centred cubic (FCC) lattice. This random
arrangement makes it energetically unfavourable for the ordered, tetragonal structure
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of sigma phase to form(How? energetically unfavourable?).
Well, in nickel-stabilised austenite, the random distribution of atoms throws a wrench
into sigma phase formation on an energetic level. Normally, chromium (Cr) and iron
(Fe) atoms are drawn together by strong attractive forces, readily forming the ordered
lattice preferred by sigma phase. Nickel (Ni), however, disrupts this "atomic attraction
party." With its different size and electronic configuration, nickel acts like an
unwelcome guest, introducing repulsive forces and hindering the formation of the
specific Fe-Cr rich regions necessary for sigma phase nucleation. This disrupts the
overall energy landscape. Creating and maintaining the ordered sigma phase
structure requires extra energy to overcome these repulsive interactions and force
atoms into specific positions. In contrast, the random arrangement in austenitic
stainless steels with high nickel content is energetically favourable. The system
doesn't have to expend extra energy to maintain this random distribution, making
sigma phase formation unfavourable.
Beyond Nickel: Additional Factors Influencing SPE Resistance
While nickel is the primary element promoting resistance, other factors can
contribute:
• Molybdenum (Mo):Mo can substitute for chromium to a limited extent in sigma
phase, potentially reducing the available chromium for sigma formation. However,
high Mo content can also have its own drawbacks, so balancing its addition is crucial.
• Nitrogen (N):Nitrogen, when present in small quantities, can also hinder sigma
phase formation by occupying interstitial positions within the lattice, further
disrupting the ordering of Fe and Cr atoms.
Immunity vs. Resistance
It's important to note that even high-nickel alloys aren't entirely immune to SPE.
With prolonged exposure to high temperatures within the critical range, even these
alloys can develop some sigma phase. However, the significantly higher nickel content
dramatically increases the incubation time and reduces the amount of sigma phase
that can form. This translates to superior resistance and a much lower risk of
embrittlement compared to conventional 300 and 400 series stainless steels.
Here's a comprehensive explanation of how sigma phase forms from the molten state
in stainless steels, incorporating both chemical and metallurgical aspects:
From Molten Metal to Delta Ferrite:
1. Solidification:During solidification from the molten state, stainless steel begins to
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form a face-centred cubic (FCC) crystal structure known as austenite (γ-austenite).
This austenite is a solid solution rich in nickel and iron atoms, with chromium and
other elements dissolved within the lattice.
2. Temperature Drop and Chromium Partitioning:As the temperature falls
below the solidification point, the solubility of chromium in austenite decreases. This
prompts some chromium atoms to come out of solution and arrange themselves in a
body-centred cubic (BCC) crystal structure called delta ferrite (δ-ferrite). This
partitioning of chromium is driven by its inherent preference for the BCC structure at
lower temperatures.
3. Chemical Composition Influence:The amount of delta ferrite formed depends on
the overall chromium content of the stainless steel. Higher chromium grades will tend
to form more delta ferrite during solidification. Additionally, elements like
molybdenum can also partition into delta ferrite alongside chromium.
Transformation of Delta Ferrite to Sigma Phase:
When the formed delta ferrite is subsequently exposed to elevated temperatures
within the sigma phase embrittlement (SPE) range (typically between 540°C and
980°C), it becomes unstable.
(Why unstable ?)
Delta ferrite becomes unstable within the SPE temperature range because the strong
affinity between chromium and iron atoms finds a more energetically favourable
arrangement in the sigma phase structure. At these elevated temperatures, the BCC
structure of delta ferrite is no longer the most stable configuration for these elements.
Driving the transformation to a more complex tetragonal structure, forming the
brittle sigma (σ) phase. The sigma phase lattice offers a lower overall energy state and
stable structure.
This transformation is driven by the strong affinity between chromium and iron
atoms finds a more favourable energetic state within the sigma phase lattice. The
transformation from delta ferrite to sigma phase depletes the surrounding austenite
of chromium. This local depletion weakens the protective chromium oxide layer on
the steel's surface, potentially accelerating corrosion in these areas.
Metallurgical Significance:
The formation of sigma phase is a diffusion-controlled process. It relies on the
movement of chromium atoms through the lattice more stable positions and
subsequently form sigma phase. This diffusion process is sluggish and takes time,
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hence the extended exposure at high temperatures required for significant sigma
phase formation. Finer grain sizes generally offer shorter diffusion paths for
chromium atoms, potentially accelerating sigma phase formation compared to
materials with larger grains. This is because shorter distances allow the chromium
atoms within delta ferrite to reach their new positions in the sigma phase lattice more
quickly.
Corrosion Implications of SPE
The formation of σ phase can have a detrimental effect on the corrosion resistance of
stainless steels. Here's how:
• Chromium Depletion:As mentioned earlier, the chromium depletion around the σ
phase weakens the passive layer, a thin film protecting the underlying metal from
corrosion.
• Stress Concentration:The presence of brittle σ phase can create localised stress
concentrations within the microstructure, increasing the susceptibility to stress
corrosion cracking (SCC).
Sigma phase embrittlement is a significant concern for engineers selecting stainless
steel for high-temperature applications. Understanding the metallurgical factors like
nickel content and δ-ferrite presence is crucial to mitigate this risk. By opting for
high-nickel alloys or controlling the δ-ferrite content, engineers can ensure the long-
term integrity and corrosion resistance of these critical components.
Take Care
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SIGMA PHASE EMBRITTLEMENT
Technical Development Engineer
February 8, 2022
Many stainless steels and other iron-chromium alloys are susceptible to a grain
boundary phenomenon known as sigma-phase embrittlement.
The major effects of this phenomenon are the loss of ductility, toughness, and
corrosion resistance, which results in the failure of the material.
The formation of the sigma phase on the material depends on the ferrite content of
the material, that is higher the ferrite content the higher the formation will be.
The sigma phase formation will be rapid in ferritic stainless steel, moderate in duplex
stainless steel, and slower in austenitic stainless steel.
CHARACTERISTICS OF SIGMA PHASE:
• Structure – Tetragonal crystal structure.
• It will higher the hardness and lower the toughness and elongation in the material.
• δ → σ – High Cr-concentrated region of δ-ferrite.
• Fastest precipitation temperature - 800°c to 850°c.
PRECIPITATION BEHAVIOUR OF SIGMA PHASE:
There are three different mechanisms that are associated with the sigma phase
precipitation in the material. These mechanisms are dependent on the type of grains
they’re precipitating in. The three different structures that the sigma phase will
precipitate are Austenite, Ferrite- Austenite interface, and delta- ferrite.
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DISSOLUTION OF SIGMA PHASE:
This formed sigma phase can be dissolved in the matrix by using the solution heat-
treatment process. With the help of the phase diagram, we can choose the
temperature needed for the material. From the iron-carbon phase diagram, above the
temperature of 1494°c for a certain period of time the σ phase will diffuse and dissolve
in the original matrix. The above process is called “σ → γ phase transformation”.
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