AN EBSD STUDY OF THE MICRO STRUCTURAL DEVELOPMENT

DURING ANNEALING OF A FOLDED SUPER DUPLEX STAINLESS

STEEL SHEET SAMPLE.
H S Ubhi1), J R Saithala2) and H Jiang1)

1) Oxford Instruments, High Wycombe. HP12 3SE. UK.

2) Fine Tubes Ltd, Plymouth, PL6 7LG UK

Abstract: Super Duplex Stainless Steels (SDSS) show complex precipitation and transformation
behavior during heat treatment processes, which affects both mechanical and corrosion properties.
This report presents some data on the microstructures that develop after folding and subsequent
precipitation during heat treatment of UNS S32750 SDSS sheet samples. The microstructural and
textural changes have been followed using SEM/EBSD techniques. Upon folding both a texture
and strain gradient form in the folded/bent region, subsequent heat treatment at 845oC results in
the ferrite phase to transform to sigma, austenite and chi phases. Transformation was found to be
accelerated by strain. Complete transformation of the ferrite phase occurred within half the
annealing time required in the unstrained regions. The local mis-orientations in the ferrite and
austenite phases reduced during annealing, however, the reduction in the austenite was not very
high and a significant amount remained even after the longest annealing time. The texture
components that developed during the folding process remained unchanged even after one hour
annealing at 845oC.
The implication of these findings could have a bearing on the formation of sigma phase during
welding of SDSS that may have residual stresses introduced during final processing.

Key words: EBSD; super duplex stainless steel (SDSS); folded strain gradient, phase
transformations.

1 Introduction

The microstructural development during the heat treatment of duplex steels has been the subject
of numerous studies [1,2,3], that have shown formation of deleterious intermetallic phases such
as sigma and chi. However, there has been little reported on the kinetics of these phases due to
strain. This study is an attempt to get some insight into this phenomenon.
In a recent study [4], the strain or local mis-orientation profiles across the bent regions in folded
sheets, were reported. The folding process introduced both, tensile and compressive gradients in
addition to texture gradients [4]. The bent regions hence provide a suitable location to study the
affects of varying strain and texture on phenomena such as recovery, recrystallisation and phase
transformations in one specimen. The current work was therefore performed on folded super
duplex stainless steel (SDSS) UNS S3270. Since the EBSD technique can easily distinguish the
various phases during the transformation of SDSS, in addition to determining in local strain and
texture, this technique has been used to follow the microstructural changes during heat treatment
of the folded specimens.

2. Experimental
SDSS sheet 1.5mm thick was folded perpendicular to the rolling direction to 90o in a press brake.
Specimens were then cut from the folded sheet and heat treated in air at 845oC for 1, 3, 6, 10, 20
and 60 minutes. The respective heat treatment profiles are shown in Figure 1a.The specimens
were then mounted in Bakelite and prepared by standard metallographic practice. Colloidal silica
was used for the final finishing step. The polished specimens were examined in a FEGSEM and
EBSD data acquired using an Oxford Instruments - Nordlys F+ detector with CHANNEL5
software. EBSD maps were collected from four regions A, C, N and T in each specimen as
illustrated in Figure 1b i.e. one away from the fold (A) and 3 from the across the fold/bent section,
i.e. compressed (C), neutral (N) and tensile(T). All data was acquired at 15kV acceleration
voltage 17nA probe current with a step size of 0.2m.

b)
a)
Figure 1. a) Heat Treatment profiles of UNS S32750 material at 845oC for various times and
b). Schematic diagram showing the 4 regions from where EBSD data was acquired.

3 Results and Discussion

The microstructures in the parent sheet and the compressed region before and after heat
treatments for 60 minutes are shown in the SEM back-scattered images in Figure 2 (a-c). The
change in microstructure is evident, but information regarding phase distribution or fractions is
difficult to discern from these images.

a) b) c)

Figure 2. SEM back-scattered images from a) parent as received sheet b) folded compressed
region and c) folded compressed region after 60 minutes at 845oC.

However, these are easily discriminated by EBSD as illustrated in the series of phase EBSD maps
in Figure 3 (a-c, d-f and g-i) from the as received, and specimens heat treated for 3 and 60.
a) d) g)

b) e) h)

c) f) i)

20mm

Figure 3. EBSD phase maps from regions C, N and T a-c) as received sheet, d-f) 3minutes and g-
i) 60 minutes at 845oC (Note colors red=ferrite, blue=austenite and green=sigma)

minutes at 845oC respectively. The variation in the phase fraction with location and time during
heat-treatment are shown in Figure 4 (a-c) and 5 (ab) respectively. It is clear from these data sets
that, while the initial ferrite fraction of approximately 50% transforms to austenite, sigma and chi
phases, the rate of the sigma phase formation in the strained regions is higher and only a small
amount of chi forms. In the unstrained regions the time for completion of transformation is about
6 minutes while it is about 3 minutes in the strained regions. The ratio of transformed austenite to
sigma is approximately 1:1, in the unstrained regions, whereas it is about 3:7 in the compressed
regions.
The variation of the mean mis-orientation in the ferrite, austenite as sigma phases during heat
treatment are shown in the EBSD maps and plots in Figures 6 and 7 respectively. These data
show that while the mean misorientation in the ferrite in the strained regions reduces with
annealing time, it does not reduce significantly in austenite and remains at the same low levels for
the sigma phase. The strain in the austenite may be due to the formation of the sigma phase as
well as slow recovery and recrystallisation in the newly formed austenite from ferrite.
The changes in texture at the bend from folding and subsequent heating are shown in Figures 8 a-
f) and g-p) in the as folded sheet and after heat-treatment for 3 minutes at 845oC. It is clear that
the texture in the as received sheet is reinforced in the tensile region, i.e. strengthening of the
{111} and {110} fibre components in the fcc and bcc phases and the rotated cube and weak {110}
fibre develop in the bcc and fcc phases in the compressed region respectively. During annealing
these texture components remain unchanged and the sigma phase develops a weak texture.
Detailed interpretation of texture development is a subject of further work.
 a) b) c)

Figure 4. a-c) Plots of % phase vs region for austenite, ferrite and sigma respectively.

a) b)

Figure 5 (a-b). Plots of % phase vs time at 845oC for the region with no strain and compression
respectively.

4 Conclusions

During annealing transformation of the ferrite phase to austenite and sigma phases was found to
be accelerated by strain. Complete transformation of the ferrite phase in the strained regions
required half the time of that in the unstrained regions. The fraction of sigma phase in the strained
regions was also higher than that found in the unstrained regions. Local mis-orientations did not
indicate completely strain free grains in the austenite phase. The local mis-orientations in the
sigma phase were low. The texture components that developed during the folding process in the
austenite were unchanged even after one hour annealing at 845oC and is the subject to further
study. The corrosion behavior of these specimens is also being investigated.

5 References.

1. Michael Pohl, Oliver Storz , Thomas Glogowski, Effect of intermetallic precipitations on the
properties of duplex stainless steel. Materials Characterization [J] 2007, 58, 6571.
2. E. M. L. E. M. Jackson, P. E. de Visser, and L. A. Cornish~Distinguishing Between Chi and
Sigma Phases inDuplex Stainless Steels Using Potentiostatic Etching. Materials Characterization
[J] 1993, 31:185-190.
3) R.A. Perren , T. Suter , C. Solenthaler , G. Gullo , P.J. Uggowitzer , H. Bohni , M.O. Speidel
Corrosion resistance of super duplex stainless, steels in chloride ion containing
environments:investigations by means of a new microelectrochemical method II. Influence of
precipitates Corrosion Science [J] 2001, 43, 727-745.
4) H S Ubhi and, H Jiang, Study of Recovery and Recrystallisation in Folded bcc, fcc and hcp
Sheet Samples, Rex & GG, [C] 2010 to be published.
a) d) g)

b) e) h)

c) f) i)

20m

Figure 6. EBSD mean mis-orientations maps from regions C, N and T a-c) as received sheet,
d-f) 3minutes and h-i) 60 minutes at 845oC

a)
b)

c)

Figure 7. a-c) Plots of mean mis-orientation vs region for austenite, ferrite and sigma phases.
a) g)

b) h)

i)
X0=N

Y0=TD
Z0=RD

c) j)

d) k)

l)

e) m)

f) n)

o)

Figure 8. Series of EBSD pole figures from a-f) ferrite and austenite phases in the as folded sheet
and g-o) ferrite, austenite and sigma phases after 3 minutes anneal at 845oC from locations C, N
and T respectively.