A p p.

7 - M i c r o s t r u c t u r e a n d p h a s e a n a l y s i s o f d u p l e x s t a i n l e s s s t e e l a fter heat treatment

H K L Technology - 2005

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Microstructure and phase analysis of
duplex stainless steel after heat treatment
Question: How can one determine the effect of Sigma and Chi phases on the
mechanical properties of duplex stainless steel samples?

Introduction
Duplex stainless steels (DSS) can contain ferrite and austenite is known to nucleate at the austenite and ferrite boundaries.
phases and have a wide range of applications where it is required The ferrite, being richer in Chromium, tends to be preferentially
both to have excellent resistance to corrosive environments and absorbed during the growth of the intermetallic phases. Elements
maintain good mechanical properties, such as in renery pipes such as Molybdenum lead to further acceleration of the formation
and off-shore platforms. The resistance to corrosion, intergranular of the intermetallic phases.
corrosion and pitting corrosion is increased by increasing the Therefore it is very useful to be able to identify the quantity of
Nickel (6-8 wt.%), Chromium (18-20 wt.%) and Molybdenum Sigma and Chi phases in the DSS. Electron back scatter diffraction
(2-4 wt.%) contents in the DSS. Corrosion along grain boundaries (EBSD) can be used to easily distinguish the various phases within
can be a serious problem, particularly after a high temperature the DSS.
treatment such as welding. This type of intergranular corrosion is
sometimes referred to as weld-decay [1].
Duplex stainless steels when heated can develop a type of
embrittlement. The effect of embrittlement can be pronounced
with increasing Chromium and Molybdenum content. The
deleterious Chromium and Molybdenum rich intermetallic Sigma
and Chi phases form between 650C and 1000C and usually
have a catastrophic inuence on the mechanical properties of DSS,
often associated with a reduction in both impact properties and
corrosion resistance [2]. Figure 1 shows a graph of the Vickers
hardness of a 2205 DSS alloy (Cr 22 wt.%, Ni 5 wt.%, Mo 3 wt.%,
N 0.2 wt%) heated at 850C up to 8 hours, where the increase
in hardness is an indication of the increasing content of the hard
embrittling intermetallic precipitates [3]. The presence of ferrite Figure 1:
greatly accelerates the formation of the intermetallic phases, which
Vickers hardness measurements for the 2205
DSS samples heat-treated at 850C as a
function of time [3].
EBSD Analysis
Table 1 shows the EBSD analysis conditions used to investigate samples of the 2205 DSS alloy, which were heated treated at 850C for
0.1, 1 and 8 hours prior to the investigation.

Table 1: Details of EBSD analysis

Sample Preparation: Mechanical polish with OPS
SEM Type: FEG-SEM
EBSD System: HKL CHANNEL5 with Nordlys II detector
Accelerating voltage: 20 kV
Probe Current: 2 nA

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H K L Technology - 2005

Results

Table 2:
List of phases investigated in the DSS alloy using EBSD.
Phase Crystal structure Lattice parameters ()
Ferrite Body Centred Cubic (BCC) a= 2.87
Austenite Face Centred Cubic (FCC) a= 3.66
Sigma Tetragonal a= 8.80, c= 4.56
Chi Body Centred Cubic (BCC) a= 8.92

In Table 2 the list of phases and their crystallographic information is shown, which were found to exist in the 2205 DSS alloy. Figure 2
shows example indexed EBSD patterns from both Sigma and Chi intermetallic phases. Figure 3 shows a fore-scatter SEM image from the
alloy heated at 850C for 1 hour and the EBSD phase map from this region is shown in Figure 4. The map clearly shows the distribution
of the different phases in this region, where the intermetallic phases are formed at the ferrite phase boundaries. The Chi phase was
found to be have higher Molybdenum content compared to the Sigma phase as shown in Figure 5.

The orientation relationships between the phases are clearly seen in the inverse pole gures shown in Figure 6. The austenite and ferrite
phases were found to have the Kurdjumov-Sachs relationship, i.e. (110)Ferrite||(111)Austenite. The Sigma and Chi phases can be seen to have
an orientation relationship with the ferrite phase, (001)Sigma||(110)Ferrite, (110)Chi||(110)Ferrite. The intermetallic phases were formed at the
expense of the ferrite phase with the increase in time of the heat-treatment, where the area fractions measured from EBSD results are
shown in Figure 7. The area fractions of the Sigma phase increased from 0.01% to 19% and the Ferrite phase decreased from 41% to
1%, as the heat-treatment time increased from 0.1 to 8 hours.

Sigma Chi

Figure 2:
Example EBSD patterns from the intermetallic phases found in the 2205 DSS alloy, which were
identied as Sigma and Chi.

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H K L Technology - 2005

Figure 3:
Fore-scatter SEM image from the duplex stainless steel sample heat treated
at 850C for 1 hour.

Figure 4:
EBSD phase map from the same region shown in Figure 3. Ferrite (Blue),
Austenite (Red), Sigma(Yellow), Chi(Green).

EBSD phase map EDS map

Figure 5:
EBSD phase map and EDS map for Mo (L) from the region highlighted in Figure 4.

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H K L Technology - 2005

Ferrite Austenite Sigma Chi

Figure 6:
Inverse pole gures for the phases in the EBSD map shown in Figure 4.

Figure 7:
Area fraction of phases measured by EBSD in the samples
heat treated at 850C for 0.1, 1 and 8 hours.

Conclusion
EBSD has been shown to be a useful tool for phase identication
in duplex stainless steels, which is particularly evident in
the analysis of the Sigma and Chi intermetallic phases. The
intermetallic phases have very little difference in chemical
composition, however they have very different crystal structures.
The EBSD results clearly show that the time of heating should be
minimised in order to reduce the formation of the intermetallic
phases which are detrimental to the mechanical and corrosion
properties of duplex stainless steels.

Answer: EBSD can be used to easily identify and measure the quantity of the Sigma
and Chi phases and help to determine their effects on the mechanical and corrosion
properties of duplex stainless steels.
References
1. R.W.K. Honeycombe and H . K . D. H . B h a d e s h i a , S t e e l s M i c r o s t r u c t u r e a n d p r o p e r t i e s, B u t t e r w o r t h - H e i n e m a n n , O x f o r d , 2 0 0 3 .
2. R.N. Gunn, Duplex stain l e s s s t e e l s M i c r o s t r u c t u r e, p r o p e r t i e s a n d a p p l i c a t i o n s, Wo o d h e a d p u b l i s h i n g L t d . , C a m b r i d g e, 1 9 9 7 .
3. J.F. Almagro, ACERINOX S. A . L o s B a r r i o s, S p a i n . P r i va t e c o m m u n i c a t i o n .
A c k n owledgement
Th i s a p p l i c a t i o n n o t e h a s b e e n w r i t t e n i n c o l l a b o ra t i o n w i t h J. F. A l m a g r o, AC E R I N O X S. A . L o s B arrios, Spain.
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