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 ele-
ments 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 composi-
tion of the conventional production heats
is shown in Figure 9(B). The same inter-
granular 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 precipita-
tion 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 con-
ventional chemical composition and the
results of the rebalanced steel, pilot scale
heat H-607. The improvement in corro-
sion values of the rebalanced steel is quite
well evident in relation to the conventional
steel and is far below the maximum al-
lowed 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 improve-
ment 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.
REM: R. Esc. Minas, Ouro Preto, 66(2), 201-208, abr. jun. | 2013 205
Development of UNS S32760 super-duplex stainless steel produced in large diameter rolled bars

A B

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
C 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)

Table 4
604 - Conventional 6.35
G-48 ass losses in the conventional
607 - Rebalanced 0.13 and rebalanced steels pilot scale
heats after 24 h at 50ºC.

Mass Loss (g/m2)

Sample Position
Individual Values Average Table 5
G-48 mass losses of 152.40 mm bar
Center of Bar End 0.06
determined in three pozsitions of the
Mid Radius of Bar Middle 0.09 0.09 ± 0.03 rebalanced steel after 24 h at 50ºC
showing values far below the maximum
Center of Bar Middle 0.12
allowed by Norsok standard of 4.0 g/m2.

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

Figure 11
Microstructure of 152.40 mm diameter
bar of rebalanced production heat (H-
7441/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 higher pitting corrosion resistance when not be only explained by the slight increase
temperature-CPT of the production compared to the conventional steel. A CPT in PREN values. Based on the metal-
conventional and rebalanced steel. It is increase of more than 20 ºC was observed. lographic evidences on pitting initiation
observed that rebalanced steel shows a The difference of CPT temperature could at the ferrite grain boundaries with Cr2N
206 REM: R. Esc. Minas, Ouro Preto, 66(2), 201-208, abr. jun. | 2013