Celso Antonio Barbosa e Alexandre Sokolowski

Metallurgy and materials

INOX 2010
Development of UNS S 32760
super-duplex stainless steel
produced in large diameter
rolled bars
Desenvolvimento do ao inoxidvel
super-duplex UNS S 32760 produzido
em barras laminadas de grande dimetro
Celso Antonio Barbosa
Engenheiro Metalurgista , Membro da ABM,
Diretor de Tecnologia e P&D ,
Villares Metals S. A., Sumar - SP, Brasil.
celso.barbosa@villaresmetals.com.br.

Alexandre Sokolowski
Engenheiro qumico, Mestre em Metalurgia,
Pesquisador Snior,
Villares Metals S.A. Sumar, SP, Brasil.
alexandre.sokolowski@villaresmetals.com.br.

Abstract
Nowadays super-duplex stainless is an important material for the Oil and Gas
industries, especially for off-shore production. In deep water exploitation the reliability
of production system is very important. Corrosion resistance for pitting of the high
alloyed duplex stainless steels with high Mo and N content has to be achieved even in
large diameters bars. Therefore, the present work deals with an improved super-duplex
stainless steel for the production of large diameter rolled 6bars up to 152.40 mm (6
inches). Among the main improvements, the corrosion resistance evaluated both by
the chemical method according to the ASTM G-48 method, as well as electrochemical
methods, was achieved. During the production of such large dimensions, the precipitation of inter-metallics and nitrides after cooling from high temperatures was studied by
changing the chemical composition using Thermo-Calc and evaluating the new proposed
chemical compositions. Several alloy compositions were laboratory scale cast, and the
austenite/ferrite balance as well as PREN pitting resistance equivalent number content
was correlated to the microstructure and the corrosion properties obtained. It was thus
possible to determine the ideal chemical composition and define the new processing
parameters to produce the UNS S32760 grade (4501) according to the Norsok standard.
The new material properties produced in a production full scale heat are also presented.
Keywords: Corrosion, super-duplex stainless steel, pitting.

Resumo
Os aos inoxidveis superduplex, atualmente, so materiais importantes para a
indstria de leo e gs, especialmente para produo off-shore. Em guas profundas,
a confiabilidade do sistema de produo muito importante. A resistncia corroso
dos aos inoxidveis duplex de alta liga com alto teor de Mo e N, especialmente em
relao corroso por pite, tem de ser alcanada, at mesmo em barras com grandes
dimetros. Portanto o presente trabalho trata de um ao inoxidvel superduplex com
propriedades melhoradas para a produo de barras laminadas de grande dimetro,
ou seja, de at 152,40 milmetros (seis polegadas). Entre as principais melhorias, a
resistncia corroso, avaliada, tanto pelo mtodo qumico, de acordo com ASTM
G-48, bem como pelos mtodos eletroqumicos, foi alcanada. Durante a produo
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Development of UNS S32760 super-duplex stainless steel produced in large diameter rolled bars

de tais grandes dimenses, a precipitao de intermetlicos e nitretos, aps o resfriamento das altas temperaturas, foi estudada atravs da alterao da composio qumica, usando o software Thermo-Calc e avaliando as novas composies qumicas
propostas. Vrias composies de ligas foram fundidas, em escala de laboratrio, e o
equilbrio austenita / ferrita, bem como o PREN, nmero equivalente de resistncia
ao pite, foram correlacionados com a microestrutura e as propriedades de corroso
obtidas. Foi possvel determinar a composio qumica ideal e definir os novos parmetros de processamento para produzir o UNS S 32760 grau (4501), de acordo com a
norma NORSOK. As propriedades dos novos materiais produzidos, em uma escala
de produo industrial, tambm so apresentadas.
Palavras-chave: Corroso, ao inoxidvel superduplex, corroso por pites.

1. Introduction
The excellent combination of mechanical strength and corrosion resistance
in various types of environments and the
good performance in applications found
in Oil and Gas fields makes duplex stainless steels (DSS) an excellent choice by
equipment designers IMOA (2009). The
development of more corrosion resistant
grades has led to the so called Super-duplex
stainless steels (SDSS), where the chemical composition is modified by increasing
specially the molybdenum and nitrogen
content, leading to a higher pitting corrosion resistance, evaluated by the pitting
resistance equivalent number PREN,
from a typical value of 35, found in normal duplex grades, to more than 40. This
new class of DSS can fight the more challenging corrosion problems found in the
nowadays deep water oil and gas reserves
where, besides temperature increases,
higher H2S and CO2 pressures are met
(Lvland, 2003). Also, besides the supermartensitic 13Cr, the SDSS shows the
best combination of corrosion resistance
and yield strength ultrapasses 600 MPa
(Barbosa, 2008). From the metallurgical

point of view and also processing characteristics, the SDSS production in large
diameters bars is a challenge because their
attractive properties may be destroyed by
the formation of precipitates due to the
more difficult thermal transfer conditions
found in bars with diameters higher than
100 mm. The most common precipitates
are chromium nitrides Cr2N and intermetallic precipitates (IP) such as sigma/chi/
phase/R phases that can be formed in the
temperature range from 600 to 1000C,
depending on the thermal cooling as well
as deformation conditions imposed during
the fabrication of large diameter bars. The
main technological properties that are adversely affected are the pitting corrosion resistance and the toughness. It is interesting
to note that in the present study, although
the pitting corrosion resistance was damaged by the presence of chromium nitrides,
the minimum impact toughness was not
affected when a very small percentage of IP
is present in the microstructure, confirming previous work showing that to have a
serious decrease in toughness several percent of IP is necessary (Nilsson & Kangas,

2007). Also important is the control of

the ferrite/austenite balance (usually near
50% each) that can be established by a
proper compositional balance between
ferrite and austenite former elements.
The knowledge of the thermodynamic
and kinetics of such complex stainless
steels is a pre-condition to understand
and control the formation of such undesirable precipitates. Many of these aspects
are very well studied and documented in
literature (DUPLEX, 2007).
In order to investigate the reasons
why corrosion resistance is sometimes
affected in the production of SDSS in
large diameter bars over 80 mm, we
conducted an extensive study in the grade
UNS S 32760 ASTM A-276 (4501), see
Table 1. The main task was to fulfill the
additional requirements found in the
Norsok standard MDS D57 Revision 3,
especially regarding pitting corrosion. The
production bars were produced by rolling
conventional cast ingots from EAF+VOD
process. After controlled rolling, the
bars were water solution annealed from
1120C.

The ingots were further forged down to

70 mm square bars with a 4:1 reduction
ratio. The chemical composition of the
produced ingots is given also in Table 1.
The conventional base composition was
reproduced in the pilot scale heat and it
is indicated as well as the modified ones.
In the rebalanced composition the PREN
number was increased via chromium and
molybdenum to more than 41. The content
of ferrite in the conventional steel, around
57%, was reduced to around 42% in the
rebalanced composition in the solution
annealing temperature of 1120C as calculated by the Thermo-Calc. The higher
amount of austenite promotes a higher

ductility and toughness (Esteban, 2008).

The specimens were cut from the
middle section of the 70 mm square bar
and exposed to pilot heats to control the
microstructure and corrosion testing. In
the production heats the samples were
taken at different positions of the 152.40
mm diameter rolled bars. The production
heats were produced by EAF+VOD and
1.7 t ingot cast. The materials were water
solution annealed from 1120C. The
specimens for corrosion testing according
ASTM G-48 method A (AMERICAN
SOCIETY FOR TESTING AND MATERIALS, 2007) and Norsok standard
were taken from the mid radius in the

2. Experimental Procedure
Pilot scale heats were produced in
order to verify the compositional effects
on the microstructures and corrosion as
well as to study the effect of the chemical composition balance. The pilot scale
heats were produced by casting 50 kg
ingots from a vacuum induction furnace,
with 140 mm medium cross section size.
All heats were cast using the same raw
material and were forged together using
the same heating condition. The chemical compositions were established using
as a base the typical composition found
in heats from regular production in order
to run the thermodynamic phase simulation using the software Thermo-Calc.

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Celso Antonio Barbosa e Alexandre Sokolowski

longitudinal direction and had the surface

polished to # 120 grit. The temperature of
testing was continuously monitored and
recorded, as can be seen in Figure 1. Also
the CPT-Critical Pitting Temperature was
determined using the potentiodynamic
method. The determination of the critical
pitting temperature (CPT) was conducted
according to ASTM G 150-99 (AMERI-

Table 1
Chemical composition of super-duplex
stainless steel UNS 32760-ASTM A276
standard (4501)), the pilot scale heats
and the rebalanced new production heat
produced (% in mass).

CAN SOCIETY FOR TESTING AND

MATERIALS, 2009) (using the same
solution recommended in ASTM G-4803, method E). All determinations were
made in duplicate. The corrosion samples
were submitted to optical microscopy
and SEM. To identify the austenite and
ferrite phases, NaOH electrolytic etchant
(20g NaOH and 80 ml distilled H 2O)

Steel

UNS S 32760

Conventional
Heat
H -7263

C
Si
Mn
Cr
Ni
Mo
N
P
S
Cu
W
PREN

Max 0.03
Max 1.0
Max 1.0
24 - 26
6-8
3-4
0.2 - 0.3
Max 0.03
Max 0.01
0.5 1.0
0.5- 1.0
40.0

0.019
0.38
0.7
24.9
6.38
3.37
0.27
0.026
0.001
0.63
0.65
40.3

was applied. Light optical microscopy

(LOM) was performed in a Zeiss inverted
microscope in the transversal specimen
direction. A 95% condence interval of
the volume fractions of ferrite, austenite
and inter-metallic phase was estimated
using manual point counting according
to the standardized ISO 9042 procedure.

Pilot Scale Heats

Conventional
(Average)
H-604

Rebalanced
H-607

Production Heat
Rebalanced
H-7441

0.02
0.42
0.69
24.8
6.54
3.37
0.28
0.026
0.001
0.64
0.65
40.4

0.017
0.4
0.6
25.3
6.85
3.68
0.26
0.026
0.003
0.6
0.7
41.6

0.024
0.35
0.6
25.3
6.84
3.55
0.25
0.017
< 0.001
0.54
0.63
41.02

Figure 1
Apparatus for determination of pitting
resistance according ASTM G-48 method
A, showing the temperature recorder of
the control thermocouples.

3. Results and Discussion

The simulations using ThermoCalc are shown in Figure 2 and 3 for the
compositions of the conventional and
the rebalanced steels. Two points should
be observed: the higher amount of austenite in the rebalanced steel, see dotted
lines in the figures corresponding to the
usual solution annealing temperature of
1120C for this grade, and the chromium
nitride precipitation is depressed to lower
temperatures (~1040C) relative to the
conventional steel(~1190C). Hot processing of super-duplex steels like rolling and

forging of large diameters bars should ideally led to conditions of finishing process
temperatures over the chromium nitride
temperature precipitation, as shown by
simulation.
Table 2 presents the amount of
ferrite predicted by Thermo-Calc and
the amount found in the samples of the
production conventional and rebalanced
steels compositions, showing a good fit.
The conventional steel showed a
high corrosion mass loss in the G-48 immersion test as can be seen in Table 3 for

three different diameter bars and heats

and with heavy presence of pitting on the
specimen surface, Figure 4.
The optical microstructure and
SEM of the corroded surfaces indicated
that the pitting initiation occurred in the
ferrite grain boundaries, Figures 5, 6 and
7. Figure 5 is the SEM examination of the
G-48 corrosion specimen surface just after
testing showing that the pitting initiation
is concentrated in the ferrite grains.
At larger magnification, as showed
in Figure 6, it was possible to observe

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Development of UNS S32760 super-duplex stainless steel produced in large diameter rolled bars

1.0
0.9
55

0.8
0.7

1
1

NPM(*)

0.6
0.5

1:T-273.15,NPM(FCC_A1#1)
2:T-273.15,NPM(HCP_A3#2)
3:T-273.15,NPM(M23C6)
4:T-273.15,NPM(SIGMA)
5:T-273.15,NPM(BCC_A2)
6:T-273.15,NPM(LIQUID)

5
5

0.4

Cr2N

0.3

44

0.2
0.1

22
3
0
800

24

1000

1200

Average:
- 50 to 54% F balance
- PREN slightly > 40
- Some Cr2N

6
1
5
6
1400

1600

TEMPERATURE_CELSIUS
6

1.0
0.9
0.8
0.7

0.6

NPM(*)

1
1

0.5

1:T-273.15,NPM(FCC_A1#1)
2:T-273.15,NPM(HCP_A3#2)
3:T-273.15,NPM(M23C6)
4:T-273.15,NPM(SIGMA)
5:T-273.15,NPM(BCC_A2)
6:T-273.15,NPM(LIQUID)

5
1

55

0.4
0.3

Figure 2
Equilibrium microstructure constituents
predicted by the Thermo-Calc software
for the conventional production steel
average composition (molar %).
Dotted line indicates the solution
annealing temperature of 1120C.
Note a predominant ferrite
microstructure is predicted.

Cr2N

0.2

0.1

2 2 24
3
2
0
800
1000

1
6
1200

5
1600

1400

Aim:
- New F/A balance
(42%F)
- Higher PREN > 41
- Nearly zero Cr2 N

TEMPERATURE_CELSIUS

Figure 3
Equilibrium microstructure constituents
predicted by the Thermo-Calc software
for the rebalanced composition (molar %).
Notice in line 2 the predicted temperature
of Cr2N is depressed to lower temperature.
Dotted line indicates the solution
annealing temperature of 1120C.

Ferrite (%)

Steel

Predicted

Real

Conventional

52

57.5

Rebalanced

42

41.3

Sample

Mass Loss (g/m2)

612 ( 127.0 mm)

10.7 / 15.6

651 ( 95.25 mm)

50.9 / 64.8

606 ( 82.55 mm)

28.1 / 67.3

Table 2
Predicted and real volume fraction of
ferrite for conventional and rebalanced
steels, at 1120C.
Table 3
Mass losses in three samples of the
conventional steel after 24 h at 50C
showing values above the maximum
allowed by Norsok standard of 4.0 g/m2.

Figure 4
Conventional steel corrosion surface
of the G 48 specimen 606 after
24 h at 50C showing the pits.

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Celso Antonio Barbosa e Alexandre Sokolowski

Figure 5
Compositional SEM image of the
corrosion specimen surface without
etching showing the pitting initiation is
concentrated in the ferrite. Longitudinal
direction. Magnification 500X.

Figure 6
Compositional SEM image of the
corrosion specimen surface without
etching showing the pitting initiation in
the ferrite grain boundaries.
Longitudinal direction.
Magnification 3,300 X.
that most of the ferrite grain boundaries
had pitting initiation. In order to identify
the presence of phases in the ferrite grain
boundaries, the same corrosion sample
was polished and etched to be observed
in the SEM. Figure 7 shows the presence
of grain boundary precipitates detected
by the compositional image (indicated
by darker points of lighter chemical elements comparative to the matrix). The
EDS profiles of such precipitates indicate
the presence of higher intensities values of
Cr and N, indicative of chromium nitride
precipitation, Figure 8.
The Figure 9(A) shows a typical
microstructure of one of the production
conventional heats showing the intensive
ferrite grain boundary precipitation of
Cr2N and the predominance of ferrite

phase with some secondary austenite.

The microstructure of the pilot scale
heat with its composition adjusted to
reproduce the average chemical composition of the conventional production heats
is shown in Figure 9(B). The same intergranular precipitation can be seen inside
the ferrite grains.
Figure 9(C) is the microstructure
of the rebalanced composition pilot scale
heat. It is clear the absence of precipitation inside the ferrite grains as observed
in the LOM.
The corrosion behavior of the pilot
scale heats were checked using also the
G-48 immersion test. Table 4 shows the
results obtained in the conventional heat
H-604 with a reproduction of the conventional chemical composition and the

results of the rebalanced steel, pilot scale

heat H-607. The improvement in corrosion values of the rebalanced steel is quite
well evident in relation to the conventional
steel and is far below the maximum allowed by Norsok standard of 4.0 g/m2.
The production rebalanced steel
showed an impressive improvement in
mass loss in the G-48 immersion test as
can be seen in Table 5 for a 152.40 mm
diameter bar tested in three different bar
positions with no occurrence of pitting on
the corrosion specimen surface, Figure 10.
The microstructure obtained in the
production rebalanced steel is presented
in Figure 11. It is evident the improvement when comparing the ferrite grains
free of precipitation and higher amount
of austenite.

Figure 7
Compositional image of SEM image
showing ferrite grain boundaries
precipitates with size less than 1.0 micron
in a polished sample of conventional steel.
Longitudinal direction.
Magnification 3,000 X.

Figure 8
Ferrite grain boundary precipitation
analyzed by EDS showing the presence of
N and Cr in the precipitate. Longitudinal
direction. Magnification 3,000 X.
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Development of UNS S32760 super-duplex stainless steel produced in large diameter rolled bars

Figure 9
Microstructure of the bars. (A) 127.0 mm diameter bar of
conventional production heat (H-7263/Sample 651) that failed in
passing in the corrosion testing ASTM G-48 showing the presence
of precipitates in the ferrite grain boundaries and the presence
of some secondary austenite, (B) conventional steel pilot scale
heat H-604 showing the presence of precipitates in the ferrite
grain boundaries and the presence of secondary austenite, (C)
rebalanced composition steel pilot scale heat H-607 showing
only the presence of ferrite with grain boundaries without nitrides
precipitates, austenite and small presence of secondary austenite.
All microstructure in the transversal direction. Electrolytic NaOH
etching. Magnification 500 X.

Pilot Heat

Mass Loss (g/m2)

604 - Conventional

6.35

607 - Rebalanced

0.13

Sample Position

Table 4
G-48 ass losses in the conventional
and rebalanced steels pilot scale
heats after 24 h at 50C.

Mass Loss (g/m2)

Individual Values

Center of Bar End

0.06

Mid Radius of Bar Middle

0.09

Center of Bar Middle

0.12

Average

0.09 0.03

Table 5
G-48 mass losses of 152.40 mm bar
determined in three pozsitions of the
rebalanced steel after 24 h at 50C
showing values far below the maximum
allowed by Norsok standard of 4.0 g/m2.

Figure 10
G-48 corrosion specimen of the rebalanced steel after 24 h at 50C showing no
pits on the testing surface.

Figure 11
Microstructure of 152.40 mm diameter
bar of rebalanced production heat (H7441/Sample 430) that passed in the
corrosion testing ASTM G-48 showing no
presence of precipitates in the ferrite grain
boundaries. Center of the bar middle.
Longitudinal direction. Electrolytic NaOH
etching. Magnification 500 X.
Table 6 shows the critical pitting
temperature-CPT of the production
conventional and rebalanced steel. It is
observed that rebalanced steel shows a

206

higher pitting corrosion resistance when

compared to the conventional steel. A CPT
increase of more than 20 C was observed.
The difference of CPT temperature could

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not be only explained by the slight increase

in PREN values. Based on the metallographic evidences on pitting initiation
at the ferrite grain boundaries with Cr2N

Celso Antonio Barbosa e Alexandre Sokolowski

precipitation in the conventional steel,

we evaluated the amount of precipitates
in both steels. Table 7 shows the Cr2N
percentages found. The rebalanced steel
showed no evidence of Cr2N precipitation
in ferrite grain boundaries both in LOM
as well as in SEM.
The relationship between Cr2N precipitation in the ferrite grain boundaries
and CPT can be seen in Figure 12. The
reduction of CPT temperature near to
50C explains why the G-48 test developed a high pitting level in the corrosion
specimens, as showed in Figure 4 and an
inacceptable mass loss, Table 3.
The PREN can be calculated using the Thermo-Calc simulation that
gives us the chemical compositions of
the equilibrium phases present in the

steel at each temperature. The chemical

composition of austenite and ferrite were
calculated in three different temperatures
including the recommended solution
annealing temperature for this steel
grade of 1120C. Figure 13 shows the
calculation results for the temperatures
of 1050, 1120 and 1200C. The first
observation is that the austenite PREN
is lower than ferrite PREN and tends
to reach the ferrite number only at high
temperatures, near 1200C. Second, the
rebalanced steel shows a PREN number
both in austenite as in ferrite higher than
the conventional steel.
As Thermo-Calc gives also the
phase molar fraction, we have also
estimated the PREN total of each steel
composition, considering only the aus-

CPT Critical Pitting Temperature (C)

Steel

Table 6
Critical pitting temperatures values
determined using potentiostatic method
of the conventional and rebalanced steels.

tenite and ferrite phases. The calculated

total PREN value is higher than 40 at
1120C for the rebalanced steel, Figure
14, showing that the compositional
changes introduced led to a good combination of stronger corrosion resistant
austenite and ferrite in a proper balance,
increasing the corrosion resistance of the
rebalanced steel.
In the Table 8 we can observe the
improvement in toughness as evaluated by
the absorbed impact energy. It is interesting to notice that the minimum required
value was obtained even in the conventional steel that failed in corrosion, showing
that the improper austenite/ferrite balance
and chromium nitride precipitation did
not deteriorate the toughness to a level
under the specified values.

Individual Values

Average

Conventional

53

55

60

56

Rebalanced

73

85

76

Table 7
Amount of Cr2N precipitated at ferrite
grain boundaries in the conventional and
rebalanced steels.

Steel

Cr2N GBP (%)

Conventional

0.84 0.14

Rebalanced

0.01

85

CPT (C)

75

65

55

Figure 12
Effect of the amount of Cr2N intergranular precipitation on the Critical
Pitting Temperature-CPT determined by
potentiostatic method (average values).

45
0,00

0,01

0,10

1,00

10,00

IP (%)

44
43
42

PREN

41
40
39
38
37

Rebalanced Austenite

36

Figure 13
Ferrite and Austenite PREN number
for the Conventional and Rebalanced
steel calculated by Thermo-Calc.

Rebalanced Ferrite

35
34
33
1040

Conventional Austenite
Conventional Ferrite

1060

1080

1100

1120

1140

1160

1180

1200

1220

Temperature (C)
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Development of UNS S32760 super-duplex stainless steel produced in large diameter rolled bars
41

PREN

40

39

38

37

Rebalanced

36
1040

Conventional

1060

1080

1100

1120

1140

1160

1180

1200

1220

Temperature (C)

Sample

Conventional (J)

Rebalanced (J)

Mid Radius ( 152.40 mm)

101.4

215.3 35.7

Figure 14
Total PREN number for the
Conventional and Rebalanced
steels calculated by Thermo-Calc.
Table 8
Longitudinal impact absorbed energy
(Charpy V) of conventional and balanced
steels at -46C (minimum required is 45 J).

4. Conclusions
The present study on large diameter
bars produced in super-duplex stainless
steel UNS S 32760 has shown that the pitting corrosion resistance can be improved
using alloy design tools like phase numerical simulation software Thermo-Calc as a
base to rebalance the alloy. It was demon-

strated that the presence of inter-granular

Cr2N in ferrite acts as a pitting initiation
reducing the critical pitting temperature
CPT of the alloy even though the mechanical properties and toughness are still
above the acceptance criteria. Besides the
alloy composition balance, the processing

parameters as finishing rolling/forging

temperatures and solution annealing
temperature are determinants to reach the
desired mechanical and corrosion properties as required by the Norsok standard
MDS D57 Revision 3 in large diameter
rolled bars up to 152.40 mm.

5. References
AMERICAN SOCIETY FOR TESTING AND MATERIALS. G 48-03: Standard
test methods for pitting and crevice corrosion resistance of stainless steels and
related alloys by use of ferric chloride solution. Annual Book of ASTM Standards.
Philadephia: ASTM, 2009.
AMERICAN SOCIETY FOR TESTING AND MATERIALS. G 150-99: Standard
test method for electrochemical critical pitting temperature testing of stainless
steels. Annual Book of ASTM Standards. Philadephia: ASTM, 2009.
BARBOSA, C. A. A contribuio das LRCs no revestimento de poos. Corroso e
Proteo, p.11-13, Novembro/Dezembro, 2008.
DUPLEX 2007. CD-ROM Proceeding. Italy: Associazione Italiana di Metalurgia,
June, 2007.
ESTEBAN, M.P. et al. Anisotropy in the mechanical properties of two duplex stainless
steels with different phase balance. European Stainless Steel Conference, p.547553, 2008.
INTERNATIONAL MOLYBDENUM ASSOCIATION (IMOA). Practical
guidelines for fabrication of duplex stainless steel. London: IMOA, 2009. 64p.
LVLAND, P. Super stainless steels. Stainless Steel Europe, p.28-37, november, 1993.
NILSSON, J. O., KANGAS, P. Influence of phase transformations on mechanical
properties and corrosion properties in duplex stainless steels. Stainless Steel World,
p.56-59, may, 2007.
Paper submitted to INOX 2010- 10th Brazilian Stainless Steel Conference, September 20-22, Rio de Janeiro, Brazil. Revised accepted December, 05, 2012.

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