Corrosion Science 70 (2013) 252–259

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Corrosion Science
journal homepage: www.elsevier.com/locate/corsci

Influence of Creq/Nieq on pitting corrosion resistance and mechanical properties

of UNS S32304 duplex stainless steel welded joints
Yiming Jiang a, Hua Tan a,d, Zhiyu Wang b, Jufeng Hong a, Laizhu Jiang b, Jin Li a,c,⇑
a
Department of Materials Science, Fudan University, Shanghai 200433, PR China
b
Research and Development Center, Baosteel Co. Ltd., Shanghai 201900, PR China
c
Institute of Metal Research, Chinese Academy of Science, Shenyang 110016, PR China
d
Nuclear Power Plant Service Company, Shanghai 200233, PR China

a r t i c l e i n f o a b s t r a c t

Article history: Pitting corrosion resistance and mechanical properties of 2304 duplex stainless steel with different
Received 16 August 2012 Creq/Nieq values after plasma-arc welding and welding thermal simulation were systematically studied.
Accepted 22 January 2013 The results showed that the lower the Creq/Nieq value in the experimental range, the better the micro-
Available online 31 January 2013
structure after welding or welding thermal cycle. High pitting resistance equivalent number in the chem-
ical composition brought in low weight loss rate and high critical pitting temperature for base metal.
Keywords: Furthermore, as the Creq/Nieq value decreased, the degradation of pitting corrosion resistance after
A. Stainless steel
welding thermal cycle reduced.
C. Welding
C. Pitting corrosion
Ó 2013 Elsevier Ltd. All rights reserved.

1. Introduction stage and without chromium nitrides. However, intermetallic

The success of modern duplex stainless steels (DSSs) is due to
their weldability as well as their excellent mechanical properties
and corrosion resistance. Compared with the earlier generation of
duplex steels, weldability has been improved appreciably, by intro-
duction of nitrogen as an alloying element and vacuum and argon
oxygen decarburization (VOD and AOD) processes. The properties
of DSS are dependent on the ferrite (a)-austenite (c) phase ratio
which in the base metal is designed to be approximately 1:1. More-
over, the precipitation of secondary phases including intermetallic
phase (r, v) and nonmetallic compounds (Cr23C6, Cr2N) has shown
a detrimental influence on the properties especially the pitting cor-
rosion resistance and toughness [1–6].
In the heat-affected zone (HAZ) and fusion zone (FZ), the micro-
structure strongly depends on thermal cycle and chemical compo-
sition. For DSS, among the parameters of welding thermal cycle,
heat input is the most important one which determines the cooling
rate of welding process directly. The lower the heat input, the fas-
ter the cooling rate. Low heat input brings on an extremely unbal-
ance microstructure with excess of ferrite phase and also results in
plenty of chromium nitrides precipitating in the interior of the fer-
rite grains or the interface of austenite and ferrite grains. Generally,
a relatively high heat input is beneficial to the microstructure of
welded joints with more austenite reformation during cooling
⇑ Corresponding author at: Department of Materials Science, Fudan University,
Shanghai 200433, PR China. Tel./fax: +86 21 6564 3648.
E-mail address: corrosion@fudan.edu.cn (J. Li).
phases are easy to form when the cooling rate is too slow, espe-
cially for the high alloyed super duplex stainless steel. Therefore,
it must be borne in mind that an upper limit to heat input is set
by the prevention of intermetallic phase precipitation, and this risk
increase with increased alloy element level [7–13].
As for the influence of chemical composition on welding of
duplex stainless steel, a great number of investigations have car-
ried out on the effect of alloying elements, especially the most
effective nitrogen [14–23]. Ogawa and Koseki [24] had pointed
out that both nitrogen and nickel could increase austenite content
of the weld, but N increase the pitting corrosion resistance while Ni
degrades the pitting corrosion resistance. Muthupandi and his
coworkers [25,26] had investigated the influence of N and Ni on
microstructure and mechanical properties of 2205 weld metals
and the results that the addition of Ni and N could significantly im-
prove the microstructure, phase balance and impact toughness, but
it seems to have no appreciable influence on the hardness of the
weld zone were obtained. Liou et al. [27,28] have carried out mean-
ingful researches to prove the beneficial influence of nitrogen on
microstructure and corrosion resistance such as pitting corrosion
and stress corrosion cracking in simulated heat-affected zones of
DSS. All these studies are focused on the influence of single alloying
element. However, a more important parameter – the ratio of chro-
mium equivalents (Creq) and nickel equivalents (Nieq), which pres-
ent the ability of stabilizing the ferrite and austenite structure from
the angle of alloying elements, was less investigated. DSS contains
ferrite stabilizing elements like Cr, Mo, Si and W as well as austen-
ite stabilizing elements like Ni, Mn, C, N and Cu. Long and DeLong

0010-938X/$ - see front matter Ó 2013 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.corsci.2013.01.037
 Y. Jiang et al. / Corrosion Science 70 (2013) 252–259 253

Table 1
Chemical composition of a series of 2304 duplex stainless steels.

Materials Concentration of alloying elements (wt.%) Creq Nieq Creq/Nieq PREN

Cr Ni Mo N Mn C Si S P Cu
2304-1 23.42 4.03 0.31 0.13 1.56 0.021 0.40 0.004 0.010 0.29 23.73 7.44 3.19 27.04
2304-2 23.54 4.60 0.31 0.13 1.67 0.011 0.41 0.005 0.010 0.31 23.85 7.66 3.11 27.16
2304-3 23.01 5.35 0.30 0.12 1.64 0.015 0.36 0.003 0.009 0.30 23.31 8.35 2.79 26.40
2304-4 23.66 4.87 0.71 0.16 1.49 0.030 0.37 0.005 0.007 0.31 24.37 9.20 2.65 29.20

Creq = %Cr + %Mo + 0.7%Nb [14]. Nieq = %Ni + 35%C + 20%N + 0.25%Cu [14]. PREN = %Cr + 3.3%Mo + 20%N [4,5].

[29,30] suggested the effect of the elements on Creq and Nieq with 2.2. Welding and thermal simulation
the following equations:
Welding was performed using autogenous PAW without filler
Creq ¼ wt:%Cr þ wt:%Mo þ 1:5 wt:%Si þ 0:5 wt:%Nb ð1Þ
metal, and the corresponding parameters were listed in Table 2.
Welding thermal cycle simulation was carried on DSS 2304 base
Nieq ¼ wt:%Ni þ 0:5 wt:%Mn þ 30ðwt:%N þ wt:%CÞ ð2Þ metal through the Gleebe 3800 thermal–mechanical simulator.
In this paper the influence of Creq/Nieq on corrosion resistance Fig. 1 shows the relationship between the temperature and the
and mechanical properties of the 2304 welded joint including the elapsed time registered by thermocouple during welding simula-
practical plasma-arc welded (PAW) joint and simulated high tem- tions. The rising rate was 350 °C/s; peak temperature was
perature HAZ has been systematically studied. A series of 2304 du- 1350 °C; holding time at peak temperature was 3 s; heat input
plex stainless steel base metal with different Creq/Nieq values has was 1.5 kJ/mm.
been chosen as the studying object and the chemical composition
of 2304 duplex stainless steel for the application was optimized 2.3. Characterization
through this study.
To observe microstructure, each specimen was electrochemi-
2. Experimental procedures cally etched by 30%KOH solution at 2 V for 15 s. The ferrite volume
fraction of the base metal, the welded joint, and the simulated high
2.1. Materials temperature HAZ was measured by Helmut Fischer MP3 Ferit-
scope. The microstructure and the morphologies after pitting cor-
Four kinds of 2304 duplex stainless steels with different Creq/ rosion were observed by both optical microscope (OM) and
Nieq value from 2.65 to 3.19, also with different pitting resistance scanning electron microscope (SEM).
equivalent number (PREN = %Cr + 3.3%Mo + 20%N), were investi- The mechanical properties such as yield strength, tensile
gated in this paper, and their composition and other important strength, and elongation of the PAW joints were measured while
information were shown in Table 1. Here the Creq and Nieq were the impact toughness of the simulated HAZ specimens was charac-
calculated used the universe formulas according to WRC 1992 Con-
stitution Diagram [17], which is more reasonable than the former
Table 2
formulas obtained by Long and DeLong in 1973 [29,30]. Welding conditions applied for PAW of duplex stainless steel DSS
2304.
Creq ¼ %Cr þ %Mo þ 0:7%Nb ð3Þ
Welding current (A) 165
Welding voltage (V) 50
Nieq ¼ %Ni þ 35%C þ 20%N þ 0:25%Cu ð4Þ
Orifice gas nozzle diameter (mm) 3.2
PREN is an experienced formula widely used to evaluate the pit- Welding speed (cm/min) 27
Nozzle height (mm) 5–6
ting corrosion resistance of austenitic stainless steels and duplex Plasma gas flow: Ar (L/min) 15
stainless steels from the angle of chemical composition. A lot of Shielding gas flow: Ar (L/min) 15
alloying elements have the influence on the pitting corrosion resis-
tance including beneficial effect and harmful effect. For example,
Cr, Mo, N, Cu, etc. have the beneficial effect while Mn, S, P, etc. have
the harmful effect. There is no universe formula for calculation of
PREN. As we known that PREN = %Cr + 3.3%Mo + x%N only consid-
ering the beneficial effect of the major three element Cr, Mo and
N, while the nitrogen factor x is in range of 16–30. Generally, x is
chosen among 16, 20 and 30. A middle value 20 is the most widely
employed to calculate the PREN value during the study for duplex
stainless steels [4,5]. They were melted in a 50 kg vacuum furnace
and then cast as a single square ingot. After removing the oxide
skin, the ingot was forged into square bloom at the temperature
ranging from 900 °C to 1200 °C and divided into several blooms
with a dimension of 150 mm  100 mm  42 mm. The blooms
were reheated at 1200 °C for 1 h and hot-rolled, using a laboratory
hot-rolling mill, into 12 mm thick plates. After hot-rolling, DSS
2304 was solution-annealed at high temperature for 12 min and
quenched in water. Due to the different chemical compositions,
the annealing temperatures for 2304-1, 2304-2, 2304-3, 2304-4 Fig. 1. Simulated welding thermal cycle curve of high temperature HAZ by thermo-
were 1020 °C, 1040 °C, 1060 °C, 1100 °C respectively. mechanical simulator Gleebe 3800.
254 Y. Jiang et al. / Corrosion Science 70 (2013) 252–259

Fig. 2. Equilibrium diagrams of 2304 duplex stainless steels with different chemical compositions obtained by Thermo-Cal software.

terized. The impact test was carried out for Charpy V-notched temperature Tf. As the Creq/Nieq value decreased from 3.19 to
specimens of 10  10  55 mm dimension at 40 °C, which was 2.65 for four kinds of 2304 DSS, both Tb and Tf increased, manifest-
a common test temperature specified for offshore application. ing that the ability of stabilizing the austenite phase was becoming
Pitting corrosion resistance of PAW joint was evaluated by stronger as it is well known that ferrite phase is more stable at high
immersing in 6%FeCl3 + 0.05 M HCl solution according to GB/T temperature.
17897-1999. After 24 h immersion, the weight loss rate was mea-
sured and the morphology was observed by OM and SEM. While 3.1. Microstructure and properties of the PAW joints
the pitting corrosion resistance of the simulated HAZ specimen
was evaluated through the potentiostatic critical pitting tempera- In Fig. 3, typical macro cross-section of the weld bead produced
ture (CPT) in 1.0 M NaCl solution according to the ASTM G150 stan- by PAW was shown. A relative wide fusion zone was formed with
dard. Since pitting of stainless steels depends strongly on the great number of large ferrite columnar grains while the austenite
surface finish, the surface of all testing specimens were ground distributed along the ferrite grain boundaries. After enlarging, the
with successive grade silicon carbide sand paper up to 1000 grit, microstructures of the fusion zone and the heat-affected zone for
degreased with ethanol, rinsed with distiller water and dried in 2304-1 (Creq/Nieq: 3.19 the largest) and 2304-4 (Creq/Nieq: 2.65
air. The test was carried out through the electrochemical station
PAR-STAT 2273 with a three-electrode cell containing a Pt foil aux-
iliary electrode and a saturated calomel electrode (SCE) as refer-
ence; all potentials quoted in this paper refer to this reference
electrode. The specimen acting as working electrode was mounted
in epoxy resin. Prior to each CPT measurement, the working elec-
trode was ground with successive grade silicon carbide sand paper
up to 1000 grit, degreased with ethanol, rinsed with distiller water
and dried in air. The CPT test was repeated at three times for the
same specimen and the average value of the results was adopted.

3. Results and discussion

Thermo-Cal software was employed to obtain the equilibrium

diagram of these 2304 duplex stainless steels and the results were
shown in Fig. 2. Two important temperatures should be paid atten-
tion to: one is the temperature at which the volume of ferrite phase
is equal to that of austenite phase, called the balance temperature
Tb, and the other is the temperature at which all the austenite Fig. 3. Macro plasma-arc welded joints cross section image of 2304 duplex stainless
transforms to ferrite at high temperature, called the ferritizing steel.
 Y. Jiang et al. / Corrosion Science 70 (2013) 252–259 255

Fig. 4. Optical plasma-arc welded joints microstructure of 2304 duplex stainless steel including fusion zone and heat-affected zone.

Table 3
Mechanical properties of 2304 base metal and PAW joints.

Materials Ferrite proportion (%) Yield strength 0.2% (MPa) Tensile strength (MPa) Elongation (%)
BM WZ
2304-1 50.9 70.0 462 645 40.0
2304-2 51.9 68.1 450 660 38.0
2304-3 48.7 61.3 443 653 36.5
2304-4 46.6 57.0 475 700 38.0

Fig. 5. Weight loss rate of 2304 base metal and plasma-arc welded joints after
immersion in corrosive 6%FeCl3 + 0.05 M HCl mixed solution for 24 h at 35 °C.
Fig. 6. SEM image of pit morphology after immersion in corrosive 6%FeCl3 + 0.05 M
HCl mixed solution for 24 h at 35 °C.
the smallest) welded joints were presented and compared in Fig. 4.
In the fusion zone, there were more and coarser austenite grains have been divided into several small parts by Widmanstatten-
existed in 2304-4 compared with 2304-1. The large ferrite grains shaped austenite apparently for 2304-4. The HAZ is a gradually
256 Y. Jiang et al. / Corrosion Science 70 (2013) 252–259

Fig. 7. Microstructure of 2304 high temperature heat-affected zone with different chemical composition.

Table 4
Volume fraction of ferrite phase in duplex stainless steel 2304 simulated HTHAZ.

Materials Direction BM HTHAZ

No. 1 No. 2 No. 3 Aver.
2304-1 Surface 52.6 69.9 71.1 71.8 70.9
Cross 51.0 67.1 63.8 64.5 65.2
2304-2 Surface 51.9 70.0 67.7 68.9 69.2
Cross 51.5 65.0 60.8 63.6 63.1
2304-3 Surface 48.7 64.9 63.1 63.4 63.8
Cross 48.0 53.5 54.4 54.5 54.1
2304-4 Surface 47.2 56.4 55.1 54.8 55.4
Cross 44.6 48.4 51.4 52.0 50.6

Fig. 9. Critical pitting temperature measured curves of 2304 high temperature

heat-affected zone according to ASTM G 150. The test condition is listed as follow:
applied potential was 0.75 V (SCE), increasing rate of solution temperature was
1 °C/min, starting temperature was 2 °C.

Table 5
CPT values of 2304 base metal and simulated HAZ.

Materials 2304-1 2304-2 2304-3 2304-4

PREN 27.04 27.16 26.40 29.20
Creq/Nieq 3.19 3.11 2.79 2.65
CPT of BM (°C) 26.5 29.0 32.0 33.5
CPT of HAZ (°C) 11.5 13.0 18.0 23.0
CPT variation (°C) 15.0 16.0 14.0 10.5

Fig. 8. Critical pitting temperature measured curves of 2304 base metal according
to ASTM G 150. The test condition is listed as follow: applied potential was 0.75 V
(SCE), increasing rate of solution temperature was 1 °C/min, starting temperature
was 2 °C.
transiting zone from fusion zone to base metal which was affected
by the thermal cycle. For duplex stainless steel, the high tempera-
ture HAZ should be emphasized on, because the most typical
 Y. Jiang et al. / Corrosion Science 70 (2013) 252–259
Fig. 10. Typical morphologies after CPT measurement for the simulated high temperature heat-affected zone specimens.
Fig. 11. Impact energy of 2304 high temperature heat-affected zone.
problems of the welded joints were associated with it. The same to
the fusion zone, more and coarser austenite grains was displayed
in HAZ of 2304-4. Moreover, it was observed that a portion of pri-
mary austenite grains of base metal were preserved in 2304-4,
while the primary austenite phase in 2304-1 has transformed to
ferrite phase totally in 2304-1 during heating stage and all the aus-
tenite phase in the high temperature HAZ was reformed during the
cooling stage of the welding process. As shown in Fig. 1, the lower
Creq/Nieq, the higher Tf value. The temperature range of single fer-
rite phase was very narrow for 2304-4 and therefore only a part of
original austenite grains dissolved into ferrite matrix during the
heating stage. On the contrary, the temperature of austenite
reforming was higher during the cooling stage, therefore, more
and coarser austenite grains precipitated.
The ferrite phase volume fraction mechanical properties of the
PAW joints were listed in Table 3. As Creq/Nieq value decreased, fer-
rite phase in weld zone was decreased gradually. However, the
mechanical properties such as strength and elongation changed
without apparent law, because the strength was not only by the ra-
tio of two phases. PAW joint of 2304-4 has the highest strength
with yield strength value equal to 475 MPa.
The weight loss rate of base metal and PAW joints for the four
kinds of 2304 DSS after immersing in corrosive 6%FeCl3 + 0.05 M
HCl solution were displayed in Fig. 5. Due to the highest PREN value
(29.20) of 2304-4 base metal had the smallest weight loss rate only
0.469 g m2 h1, representing the best pitting corrosion resistance.
Other three kinds of 2304 base metal exhibit similar pitting corro-
sion resistance. From 2304-1 to 2304-4, the weight loss rate of the
welded joint was decreased as the Creq/Nieq value decreased gradu-
ally. 2304-4 welded joints presented the best pitting corrosion resis-
tance too. Pit morphology of 2304-1 PAW joints after immersion was
shown in Fig. 6 as the typical. It was easily found that the coarse
ferrite grains have been corroded and the Widmanstatten-shaped
austenite grains retained, demonstrating that the ferrite phase was
257
less resistant than the austenite phase, which has also been proved
by a great number of former studies [31–34].
3.2. Microstructure and properties of the simulated HAZ
Fig. 7 shows the microstructure of simulated HAZ of four kinds
of 2304 DSS after the same welding thermal cycle in Fig. 1 through
Gleebe 3800 thermal–mechanical simulator. A part of primary aus-
tenite phase in 2304-3 and 2304-4 existed in high temperature
HAZ apparently, especially in 2304-4, resulting from the lower
Creq/Nieq value. The ferrite phase volume fraction of base metal
and simulated HAZ on the surface and cross section for four kinds
of 2304 DSS were summarized in Table 4. As the Creq/Nieq value de-
creased, the ferrite phase content decreased both in base metal and
HAZ. The ratio of ferrite phase and austenite phase in 2304-4 HAZ
was near 1:1 and presented a more balanced microstructure.
Typical CPT curves of base metal and simulated HAZ were shown
in Figs. 8 and 9. The detailed CPT values were summarized in Table 5.
The same to the weight loss rate of welded joints, 2304-4 exhibited
the best pitting corrosion resistance for both base metal and HAZ
with the highest CPT values. Generally, the higher the PREN value,
the better the pitting corrosion resistance for duplex stainless steels
or austenitic stainless steels. In this paper, the results were not al-
ways consistent with this 2304-3 with the lowest PREN value
(26.40) possessed the second high CPT value among the investigated
four materials. There were two possible causes. One was the nega-
tive effect of harmful chemical elements such as P, S was not consid-
ered during the calculation of PREN value. Apparently the P, S in
2304-3 was lower than those in 2304-1 and 2304-2. The other was
the pitting corrosion resistance of multi-phase alloys was dependent
on the weakest phase. It was demonstrated that pitting corrosion
resistance of duplex stainless steels had been determined by PREN
value of the weaker phase not that of the whole alloy, since the Cr
and Mo enriched in ferrite phase, while Ni and N were concentrated
in austenite phase. Solution-annealing heat treatment was a key
process that not only adjusted the two phase ratio but also modified
the distribution of major alloying elements between two phases.
Annealing temperature should be differed from each other for the
investigated four 2304 duplex stainless steels due to the different
chemical composition, and the equilibrium diagrams obtained by
Thermo-Cal software had proved this. Due to different annealing
temperature, The PREN of weakest phase in 2304-3 may be higher
than that of 2304-1 and 2304-2, although PREN of 2304-3 was a little
lower than that of 2304-1 and 2304-2.
Compared with the base metal, all the HAZ specimens showed
impaired pitting corrosion resistance with a drop of CPT value more
than 10 °C, especially for 2304-1 and 2304-2. The decrease of pitting
corrosion after welding process or welding thermal cycle for duplex
stainless steel is resulted from two aspects of the microstructure
evolution during welding, one is the lower chromium and molybde-
num content of ferrite phase in heat-affected zone or fusion zone
compared with parent metal; the other is the precipitation of Cr2N
258 Y. Jiang et al. / Corrosion Science 70 (2013) 252–259
in the ferrite phase [7,15,34–36]. It was worthy to pay attention to
the variation of CPT and the Creq/Nieq value of the four 2304 DSS.
The lower the Creq/Nieq value, the less the degradation of pitting cor-
rosion resistance after welding. Among the investigated four 2304
DSS, the drop of pitting corrosion resistance after the same welding
thermal cycle was the least for 2304-4, which indicated that 2304-4
possessed the best weldability properties from the angle of the cor-
rosion resistance. The typical pit morphologies after CPT test were
displayed in Fig. 10. Ferrite phase was less resistant for the simulated
HAZ specimens and pitting occurred at ferrite grains, which agreed
with the previous investigations [15,17]. Besides the pitting corro-
sion resistance, the impact toughness was another important
property significantly affected by welding process for duplex
stainless steel. Fig. 11 shows the impact energy of the 2304 duplex
stainless steel simulated HAZ. Different from the pitting corrosion
resistance, the impact energy of 2304-3 was the highest among four
kinds of duplex stainless steel, the other three kinds of HAZ showed
similar impact energy. After systematical consideration on pitting
corrosion resistance, impact energy, microstructure phase balance,
2304-4 was chosen as the optimum chemical composition for
2304 duplex stainless steels.
4. Conclusions
The major conclusions were drawn as follows:
1.
Creq/Nieq has a decisive influence on the microstructure of welded
joint and simulated high temperature HAZ. The lower the Creq/Nieq
value, the more the austenite phase formed after welding or ther-
mal cycle and the microstructure was more balanced.
2.
The drop of pitting corrosion resistance after welding or welding
thermal cycle was closely related to the Creq/Nieqvalue. The drop
increased as the Creq/Nieq value increased and the composition
with lower Creq/Nieq value showed better weldability from the
angle of pitting corrosion resistance.
3.
With systematical consideration of the mechanical properties, cor-
rosion resistance, microstructure phase balance, 2304-4 was cho-
sen as the optimum chemical composition for application of
2304 duplex stainless steels at last.
Acknowledgements
The authors would like to thank Gang Hu for his great help with
SEM characterization, whilst gratefully acknowledge the helpful
collaboration of Baosteel. This work is supported by the National
Science Foundation of China (Grant Nos. 51131008, 51134010
and 51071049).
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