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ISIJ International, Vol. 48 (2008), No. 11, pp.

15961602

Microstructural Evolution during Industrial Rolling of a Duplex


Stainless Steel

G. FARGAS,1) N. AKDUT,2) M. ANGLADA1) and A. MATEO1)

1) Dept. Cincia dels Materials i Enginyeria Metal.lrgica, Avda. Diagonal 647, Universitat Politcnica de Catalunya, 08028,
Barcelona, Spain. E-mail: antonio.manuel.mateo@upc.edu 2) OCAS N.V./Arcelor Research Industry Ghent, ArcelorMittal
Group, John Kennedylaan 3, B-9060, Zelzate, Belgium.
(Received on April 16, 2008; accepted on August 4, 2008 )

The microstructural evolution of a duplex stainless steel EN 1.4462 during the industrial rolling process
has been examined. The ferritic and austenitic phases were analyzed separately after each rolling and an-
nealing step. Optical microscopy and transmission electron microscopy, together with texture measure-
ments, have been used to characterize the morphology and the preferred crystallographic orientations of
both phases. Additionally, the hardness evolution in ferrite and austenite after each industrial step was
measured by instrumented indentation. The results show that microstructural features observed after hot
rolling tend to remain during further processing and they are essentially present in the final cold rolled and
annealed product.
KEY WORDS: duplex stainless steel; rolling; annealing; texture; anisotropy.

erations like deep drawing. Therefore, the study of the mi-


1. Introduction
crostructural changes and texture evolution during the dif-
Duplex stainless steels (DSS) have a microstructure ferent stages of the rolling process is important in order to
where ferrite and austenite are present in approximately understand their influence on the properties of the final in-
equal amounts. The industrial interest on this stainless steel dustrial product. Both, the hot and the cold working behav-
grade arises from its attractive combination of mechanical iour of the steel have to be analysed, together with the in-
properties and corrosion resistance, which are better than vestigation of the restoration mechanisms active during the
predicted by the law of mixture. As a consequence, DSS annealing treatments.
exhibit an overall performance unattainable neither for The hot forming behaviour of austenitic and ferritic
austenitic nor for ferritic stainless steels.15) stainless steels has been widely characterized mainly by
Due to their properties, DSS today are being mainly used means of hot torsion and compression tests.13,14) From these
in the off-shore, chemical and petrochemical industries, e.g. studies, it is well known that ferrite and austenite behave
for marine constructions, ships outer skins, pipelines and differently during plastic deformation. During hot working
power plants.69) DSS are mainly used in form of flat prod- the two major mechanisms of restoration of metals are
ucts but cast structures for e.g. off-shore applications exist dynamic recovery (DRV) and dynamic recrystalization
as well. The processing route to manufacture DSS sheets (DRX), whereby the stacking fault energy (SFE) dictates
generally consists in alternative steps of rolling and anneal- which mechanism will take place. While single-phase
ing, as presented in Fig. 1. austenitic stainless steels can undergo DRX due to their low
After continuous casting, the slab is hot rolled in several SFE, in ferritic stainless steels, which have a much higher
passes in order to attain large thickness reduction. Then, the
material is annealed to recover the ductility for the subse-
quent cold rolling up to the required final thickness. The
process ends with a final annealing which gives the steel
product the appropriate characteristics for future applica-
tions. During these industrial process steps the steel under-
goes microstructural changes, which affect the mechanical
properties of the final product. Since during rolling both
phases align in the rolling direction (RD), the microstruc-
ture becomes morphologically anisotropic and even marked
crystallographic textures can appear. As a result, their me-
chanical properties are strongly direction dependent1012) Fig. 1. Schematic sketch of the industrial processing route for
and this often gives raise to problems for sheet forming op- (duplex) stainless steels.

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SFE than austenite, DRV is more likely to occur. However, Table 1. Chemical composition (in weight-%) of the studied
in the latter case, conditions that hinder DRV and favour the duplex stainless steel EN 1.4462.
onset of DRX are also possible.
The simultaneous presence of both phases in DSS makes
the situation more complex. There are only a few studies in
literature dealing with high temperature deformation of It was supplied after each of the four different industrial
DSS in which controversial results about the austenite be- process steps indicated in Fig. 1. The chemical composition
haviour are presented. Some authors indicate that DRX of the alloy is given in Table 1.
takes place15,16) but others suggest that this mechanism is The first condition studied was the hot rolled steel (at the
inhibited in these two-phase alloys.1719) Concerning ferrite, end of the finishing mill), from now on designated as HR,
Cizek and Wynne20) described its softening as an extended which was supplied in the form of plates of 300400 mm
dynamic recovery, while other authors called it continu- and a thickness of 6 mm. The industrial hot rolling schedule
ous recrystalization.21) The difference between these two followed to obtain these plates consists basically in two
mechanisms is defined in terms of the relative amounts of steps. First, cast slabs of 250 mm of thickness are reheated
low and high angle boundaries in the microstructure.22) to 1 250C and subsequently pre-rolled to a thickness re-
Another factor to consider is that during deformation, duction of 25% (150 mm). Before second step, the slabs are
both at high temperature and at room one, the strain parti- cooled down to room temperature and their surface is
tioning between the two phases is not homogenous. Mainly ground. The final rolling operations starts with a reheating
it is influenced by many phenomena such yield point and at 1 250C and then slabs are rough rolled with a total
strain hardening of each constitutive phase, volume fraction thickness reduction of 80%, i.e. from 150 to 30 mm thick-
and phase morphology. A recent study concerning hot ness. Subsequently, the rough rolled sheets are hot rolled
workability demonstrates that ferrite accommodates three with the final 6 mm thickness which corresponds to a total
to five times more strain than austenite.23) This result was reduction of 96%. Typical finishing temperatures are be-
obtained by measuring the length, width and height of the tween 975C and 1 000C. Next, the sheets are rapidly
austenite grains after hot rolled quenched samples. It was cooled to 650C by means of water sprays in the run out
considered that strain partitioning between the two phases table and coiled. The second supplied condition was after
results in translations of the austenite grains in the continu- hot rolling and annealing (HRA) at a temperature of ap-
ous ferrite matrix. At room temperature, the microstructure proximately 1 080C for around 15 min and the third condi-
of cold worked DSS is generally characterized by formation tion was after cold rolling (CR). In this case the sheet
of dislocation cells in ferrite, whereas a much more uni- (600150 mm) had a thickness of 2 mm. The last one was
form dislocation distribution with high incidence of stack- the final product (FP) of the industrial process obtained
ing faults is found in austenite.24) In this condition, both after the last solution annealing treatment at 1 050C for
hardness and dislocation density are higher in austenite, app. 10 min. The sample dimension was equal to the one
which is the phase that exhibits more strain hardening and after CR.
stored energy.2426) The microstructures were examined by both optical and
The dynamic and static mechanisms that develop during transmission electron microscopy (TEM). For optical mi-
annealing are even more complex because they are not croscopy, electrolytic etching in KOH solution was used.
arising to the same extend as for monophasic ferritic and This etching leaves ferrite grains in brown colour and
austenitic stainless steels. Among others, factors such as austenitic ones in white.
the volume fraction of each phase and the nature of the in- A detailed crystallographic characterization was carried
terphase will determine the softening processes during an- out using a SIEMENS D5000 texture goniometer. Incom-
nealing in such duplex structures. Generally, extensive re- plete pole figures were measured in the back reflection
covery takes place in ferrite on annealing and also recrys- mode at the centre layer of the rolling sheet. Thereby, for
talization nuclei are formed. The preferred areas for recrys- the ferritic BCC phase the {110}, {200}, {211} and {310}
tallization nucleation are regions with high density of shear pole figures were obtained, while for the austenitic FCC
bands. Recrystallization in austenite occurs in a more dis- phase the {111}, {200}, {220}, and {311} pole figures
continuous mode, preferentially at ferrite/austenite inter- were recorded. Subsequently, the orientation distribution
faces, deformation twins and shear bands.24,2729) functions (ODF) for both phases were computed. Tradition-
Most of the works available in the literature concern the ally, the ODF is represented in sections j 2constant for the
behaviour of DSS under specific thermomechanical condi- FCC and j 1constant for the BCC phase in steps of 5.
tions, i.e. hot deformation, cold deformation or static an- Hardness was measured in both phases after each process
nealing. The aim of this paper is to give an overview of the step at the central layer of the rolling sheet. Because of the
microstructural evolution of DSS during the whole indus- small thickness of the austenite and ferrite layers, hardness
trial rolling process, where the material is submitted to dif- tests were made with a MTS Nanoindenter XP instrument
ferent states and to study the influence on the mechanical with a Berkovich indenter at constant deformation rate of
properties and on formability of the final industrial product. 0.05 s1 up to 500 nm of indentation depth. The hardness
values were obtained by the method developed by Oliver
and Pharr.30)
2. Experimental Procedure
Tensile testing of the final industrial product was carried
The material studied was a duplex stainless steel EN out at room temperature using an INSTRON 5585 comput-
1.4462 produced by UGINE & ALZ (ArcelorMittal Group). erized universal testing machine equipped with two exten-

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ISIJ International, Vol. 48 (2008), No. 11

someters, i.e. in the direction of the tensile stress and per-


pendicular to it, to measure plastic-strain ratios (r-values)
according to ASTM E517-81.31) The tests were performed
on samples machined at 0, 45 and 90 to the rolling direc-
tion (RD), i.e. longitudinal (L), diagonal (D) and transver-
sal (T), in order to determine mean anisotropy (r) and pla-
nar anisotropy (Dr) by using the following two equations:

(r02r45 r90 )
r ..........................(1)
4
(r0 r902r45 ) Fig. 2. Three-dimensional microstructure of the hot rolled du-
r  .........................(2)
2 plex stainless steel.

To prove the influence of planar anisotropy on the forming


properties of the sheet, earing tests according to ISO
1153132) were carried out with a punch diameter of 20 mm
and using circular samples with a diameter of 40 mm.

3. Results and Discussion


3.1. Microstructural Evolution
As a result of the rolling process, the steel in the HR con-
dition shows already a strongly oriented microstructure
which is aligned in the rolling direction RD (Fig. 2). A
characteristic pancake-like microstructure was observed
consisting of flattened, widened and elongated austenite and
ferrite bands, whose thicknesses (dimension in the normal
Fig. 3. TEM micrograph of the hot rolled duplex stainless steel.
direction ND) were between 0.5 and 11 m m for both phases.
In the rolling plane, ferrite appears with very irregular mor-
phology and wavy boundaries as a consequence of being
the phase which carries most of the deformation, as demon-
strated by Duprez23) since the ferritic phase is not only the
matrix phase but also the softer phase. For the HR condi-
tion, TEM observations revealed a structure of subgrains in
ferrite (Fig. 3) due to the extended dynamic recovery,20)
which is similar to the continuous recrystallization that
takes place in ferritic steels during deformation at high
temperatures.21) Through the recovery process part of the
dislocations are annihilated. The remaining dislocations are
stored in low-angle dislocation walls resulting in the forma-
tion of subgrains. The merging of these dislocations walls Fig. 4. Microstructure of the hot rolled and annealed duplex
leads to a gradual build up of misorientation between stainless steel.
neighbouring subgrains. Austenite appeared with a higher
grain size than ferrite as a result of dynamic recrystalliza- anisms had started to act during hot rolling. During the an-
tion and/or metadynamic recrystalization, which can take nealing process extensive recovery took place in ferrite
place during the cooling of the plate from hot rolling. In with an increase of the average size of the subgrains (Fig.
austenite, which has a low SFE, dislocations are less mobile 5). As it can be observed, the recovery is affected by the
and dynamic recovery is limited. Consequently, once a crit- orientation present after deformation and, as a result, sub-
ical strain is exceeded, the driving force becomes large grains develop following the rolling direction.
enough for dynamic recrystallization when the dislocations There is a marked reduction in the thickness of the layers
are eliminated through the replacement of deformed grains at the end of the cold rolling step, leading to values between
by new dislocation-poor grains. 3 and 5 m m. In almost all observations of the material in the
After the subsequent annealing at 1 080C, the mi- CR condition, ferrite and austenite layers are essentially
crostructure of the HRA material is shown in Fig. 4. For one grain thick, so the layer spacing may be considered as a
this condition, the longitudinal section presents layers of good approximation to the grain size in this section. As a
austenite and ferrite with thickness between 3 and 11 m m. consequence of (shear) deformation, flattened broken bands
In the rolling plane, the wavy morphology of ferrite has al- of austenite and ferrite are visible at the rolling plane (Fig.
most disappeared and the microstructure is, compared to 6).
the HR material, characterized by thicker bands of austenite After the last annealing step at 1 050C, softening mech-
and ferrite. TEM observations of austenite did not differ anisms lead to a final industrial product, which recovers the
considerably from the HR step because the softening mech- aligned phases along the rolling direction originated in the

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Fig. 8. TEM micrograph of the final industrial product: a) Ferrite


and b) Austenite.

Fig. 5. TEM micrograph after industrial hot rolling and anneal-


ing.

Fig. 6. Three-dimensional microstructure of the industrially cold Fig. 9. Variation of austenitic phase volume fraction after each
rolled duplex stainless steel. industrial process step.

3.2. Texture Evolution


In Figs. 10 and 11, the texture development of the ferritic
and austenitic phase during the different industrial process
steps, i.e. HR, HRA, CR and FP, is shown. Textures appear
with a marked intensity in ferrite, mainly consisting of
sharp a -fiber (110//RD) spread from {001}110 to
{112}110 (Fig. 12(a)). The a -fiber exhibits a similar sta-
tistic relevance in the final industrial product and in the hot
Fig. 7. Three-dimensional microstructure of the final industrial rolled plate. Orientation density values along a -fiber show
product. a maximum on the {001}110 orientation for all the stud-
ied conditions (Fig. 10). An interesting feature is the weak-
first stage of the industrial process (Fig. 7). For the FP a ness of the {111}110 orientation, just like for the rest of
subgrain structure of ferrite is not observed anymore by the g -fiber components (Fig. 12(a)) which usually are the
TEM (Fig. 8). The main part of the new grains formed dur- dominating textures for BCC metals after rolling and an-
ing annealing is equiaxial and they have a low dislocation nealing. This result is in agreement with the previous stud-
density. This feature is also visible for austenite, where the ies carried out with duplex stainless steels.2933)
presence of annealing twins is the main feature. In the austenite, texture of HR steel is well defined (Fig.
The variation of the austenitic phase volume fraction 11(a)). The main part of the deformation rolling textures
during the industrial process is shown in Fig. 9. As it can be characteristic of FCC metals are observed (Fig. 12(b)),
seen, HR steel presents the lowest volume fracture of i.e. Brass ({011}211), Copper ({112}111) and S
austenite percentage compared with the rest of the studied ({123}634) orientations, lying on the b -fiber, which is
conditions. For hot rolling, the steel first becomes re-heated close to the g -fiber, and the Goss ({011}100) component.
at high temperatures (1 250C) before HR. In this high tem- Moreover, the presence of cube texture reveals that during
perature range the ferritic phase is more stable and less the hot rolling step, austenite recrystallizes dynamically
austenite is present. Industrial annealing conditions, after and/or meta-dynamically, i.e. when rolling deformation is
hot and cold rolling, proceed at lower temperatures and stopped but temperature is still elevated; nuclei grow into
therefore phase transformation of ferrite to austenite is en- the heterogeneous ferritic matrix, which is partly dynami-
hanced. Note that the little drop in austenite volume frac- cally recrystallized. That a dynamic recristallization and de-
tion after CR might be related to the deformation induced formation occur simultaneously is noticeable by the RD-ro-
austenite to a -martensite transformation, which retrans- tation of the cube orientation via the Goss to the Brass ori-
forms to austenite again after the final annealing process. entation, which is the ultimate deformation component in

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Fig. 10. Texture development of the ferritic phase after each industrial processing step: Fig. 11. Texture development of the austenitic phase after each industrial processing step:
a) HR, b) HRA, c) CR and d) FP. a) HR, b) HRA, c) CR and d) FP.
ISIJ International, Vol. 48 (2008), No. 11

Fig. 13. Austenite and ferrite hardness measured after each in-
dustrial process step.

Table 2. Tensile test results of the final industrial product.

Fig. 12. Selected ODF sections with some important fibers and Table 3. r-values obtained from the tensile test of the final in-
orientations: a) BCC metals and b) FCC metals. dustrial product.

FCC materials with a low stacking fault energy.34) This RD-


rotation of the cube orientation manifests itself in different
intensities in all processing steps, see Fig. 11. In addition,
in the course of processing the Copper orientation shifts a similar degree, being the hardness of the austenite higher
from its ideal position (j 190) to lower j 1-values, which than that of ferrite due to the nitrogen addition and the low
is an indication for deformation inhomogeneities like shear stacking fault energy. Analogous results were reported by
deformation and the formation of shear bands. other authors2426) by measuring the hardness with increas-
It is also worth mentioning that the texture intensity de- ing plastic deformation. They observed that at room tem-
creases after each process step. This is due to the fact that perature austenite displays more strain hardening than fer-
after each annealing the new recrystallized grains adopt rite with a considerable increase of dislocation density. At
random orientations. The texture intensity is the highest the end of the industrial process, the difference in hardness
after HR because of the elevated temperatures, where orien- between austenite and ferrite remains similar to that ob-
tation rotations in austenite and ferrite are easier than dur- served after cold rolling, despite both phases have softened
ing cold rolling. The similarity between the ferritic texture significantly as a consequence of the recrystallization
of the FP and the HR conditions results from the fact that, process that takes place during the last annealing step.
at high temperatures, ferrite is the softer matrix phase, and
therefore it carries out most of the deformation. As a conse- 3.4. Anisotropy Evaluation of the Final Industrial
quence, ferrite develops the same type of texture and inten- Product
sity as after HR. For the same reason the ferritic matrix has The results obtained from the tensile tests are summa-
higher texture intensities than the harder austenitic second rized in Table 2. The anisotropy is clearly reflected on me-
phase. chanical properties considering the three orientations of the
rolled sheet, i.e. L (0), D (45) and T (90). It can be seen
3.3. Hardness Evolution that the highest values of yield stress (s y) and ultimate ten-
The hardness evolution of both phases during the differ- sile strength (s uts) corresponded to the transversal direc-
ent steps of the process is shown in Fig. 13. At the end of tion, while diagonally orientated samples exhibited the
the hot rolling process ferrite is harder than austenite. As lowest strength but the highest ductility. This marked
demonstrated in other studies,23) when duplex stainless steel anisotropy may have a negative effect for applications be-
is deformed at high temperatures most of the strain is taken cause usually the direction of the applied stresses in indus-
by ferritic matrix which flows around austenite grains. In trial uses corresponds with the rolling direction as a result
that way the authors also considered that this difference in of the limited width of the flat product.
strain partitioning lead to a considerable incompatibility in This strong directionality is also noticeable with the r co-
strain between the a /g at the phase boundaries which was efficient, which has the maximum value at 45 and de-
supposed to be assume mostly by the ferrite. After the sub- creases drastically for samples tested at 0 and 90 with re-
sequent annealing step, an extended recovery process leads spect to the rolling direction (Table 3). The calculated
to a considerable decrease of ferrite hardness. In contrast, mean anisotropy (r) is inferior to one, indicating that the
hardness of austenite remains unchanged as a consequence strength in the thickness direction is lower than the average
of the softening initiated in the preceding hot rolling step strength in the directions in the plane of the sheet and, as a
which reduces the driving force for recrystallization. Dur- consequence, this material will exhibit limited formability
ing cold rolling both phases experienced strain hardening in by deep drawing.

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ISIJ International, Vol. 48 (2008), No. 11

The authors owe their gratitude to ALZ (today UGINE &


ALZ, ArcelorMittal Group), for providing the material via
OCAS (today Arcelor Research Industry Ghent, Arcelor-
Mittal Group), to OCAS for carrying out the texture meas-
urements and to the Technologic Center of Manresa for its
technical support in forming tests.

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