Paper No.

10512

Effects of nitrides precipitation in duplex stainless steel

Marco De Marco, Marco Palombo Anthony Pianezze, Abderrahmane Taiche

IIS Esirem Dijon – Ecole d’Ingénieurs,
Lungobisagno Istria, 15 - 16141 University of Bourgogne, 9 Avenue Alain
Genova, Italy. Savary, 21000 Dijon, France

Valentina Spinelli, Marina Delucchi

DICCA - Università degli Studi di Genova,
P. le J. F. Kennedy, 1 - 16129 Genova,
Italy.

ABSTRACT

Duplex Stainless Steels (DSS) are characterized by a dual-phase ferritic-austenitic microstructure and exhibit
high corrosion resistance and excellent mechanical properties. However, formation of different types of
intermetallic phases and precipitated compounds may occur during fabrication processes such as welding,
hot working and heat treatments; this can influence toughness and corrosion resistance. With regard to this,
some material standards/specifications (NACE, NORSOK, Company standards) introduced certain
requirements for the precipitates content (e.g. sigma phase, chromium nitrides) in the DSS microstructure.
However, these limits can deviate from the accuracy/capability of the most common counting methods (e.g.
Light Optical Microscope-LOM) point-counting, scanning electron microscope (SEM)-counting, image
analysis using dedicated software), especially for very fine and interspersed phases such as nitrides.
The aim of this paper is to find a correlation between nitride content/distribution and properties of two of the
largely adopted DSS, UNS S32205 and UNS S32750. In order to verify the detrimental effects on corrosion
and toughness of the nitride precipitation (NP), pitting corrosion tests and Charpy-V impact tests and fracture
mechanics tests were carried out on different simulated bulk specimens.

Keywords: Duplex Stainless Steel, Corrosion, Chromium Nitrides, Oil & Gas, Pitting, Fatigue, Toughness.

INTRODUCTION

The chemical composition and microstructure of Duplex Stainless Steels (DSS) determine the corrosion
resistance and excellent mechanical properties.1 The microstructure of a material can be altered after a
thermal or mechanical treatment resulting in new properties.3-9

The precipitation of different types of intermetallic phases in DSS can occur during fabrication processes
such as welding, hot working and heat treatments. Furthermore, in most applications of the two most widely
used DSS, UNS N° S32750 and UNS N° S32205, precipitation of intermetallic phases could induce a
decrease in toughness and/or corrosion resistance (e.g. marine applications, oil and gas industry equipment,
flue gas desulfurization equipment, chemical process pressure vessels, piping and heat exchangers). 3,9,14

©2018 by NACE International.

Requests for permission to publish this manuscript in any form, in part or in whole, must be in writing to
NACE International, Publications Division, 15835 Park Ten Place, Houston, Texas 77084.
The material presented and the views expressed in this paper are solely those of the author(s) and are not necessarily endorsed by the Association.
1
 Therefore, some material standards/specifications, especially in the oil and gas industry (NACE(1),
NORSOK(2), and other specifications), introduced some specific requirements for those phases that are
detrimental to the material properties (e.g. sigma phase, chromium nitrides). 10,11

However, in certain cases these limits can deviate from the accuracy/capability of the most common counting
methods (e.g. Light Optical Microscope (LOM)-point-counting, Scanning Electron Microscope (SEM)-
counting, image analysis by dedicated software), particularly for very fine and interspersed phases such as
intragranular quenched-in chromium nitrides.

Quenched-in chromium nitrides are small nano-sized (until 10 nm) particles that appear as clouds into ferrite
grains (intragranular). They are typical of high temperature (T> 1100 °C) treatment and fast cooling rates (as
in the case of welding). The precipitation is caused by lack of diffusion of Nitrogen from ferrite to austenite
and N2 supersaturation of ferrite; Cr2N precipitate as small scattered particle in ferrite phase

The purpose of this paper is to correlate the effects of the latter precipitates to the mechanical and corrosion
resistance properties.12,13

In this work, simulated precipitation was carried out using heat treatments at 1200°C followed by cooling at
different rates using water, oil and air as the cooling media. Two different DSS alloys were investigated, UNS
S32750 and UNS S32205, and the material characterization was carried out by Charpy-V impact tests (CVN)
together with a pitting corrosion test in ferric chloride solution and hardness measurements. Lastly, the
microstructures of the specimens were examined by LOM.

EXPERIMENTAL

The heat treatment was carried out in a furnace at 1200°C for 1 hour, heating all the specimens together. In
order to obtain different cooling rates, each specimen was extracted from the furnace and put in a different
cooling media (water, oil and air). The specimens were labelled adding the suffix –A. –O or –W respectively
for the air, oil or water cooling media.

The dimensions of the heat treated specimens were 60X60X10 mm.

For the examination of the microstructures, the specimens were polished and a double electrolytic etching
was subsequently performed in order to detect the presence of precipitated phases. The first etching was
carried out in a 10% oxalic acid solution at 6V for 5-8 sec (ASTM(3) E407 etchant No. 13)15 with the second
etching in a 20% NaOH solution at 4V for 5-8 sec (ASTM E407(3) etchant No. 20)15. The microstructures
were observed with a LOM.

The Vickers hardness indentations were performed and measured using an automatic Struers Duramin A-
300 Macro-Indenter and with a load of 10 kgf (HV10). The impact toughness tests were performed on Charpy
V-notched specimens at a temperature of -46°C.

The corrosion pitting test was performed in accordance with ASTM A923(3) and NORSOK(2) ST M601
respectively for the 2205 and the 2507 specimens. The specimens were kept in a ferric chloride solution for
24 hours with a solution at a temperature of 25°C for the 2205 specimens and 40°C for the 2507 specimens.
Each sample was finished up to 120 grit and later subjected to pickling for 1 hour in a solution of 82% water,
15% nitric and 3% hydrofluoric acid at 60°C. After the tests, an optical stereo-microscope was adopted for
searching for the presence of pitting on the specimens.

The chemical compositions of the DSS were detected through an optical emission spectrometer.

The determination of fatigue crack growth rates (FCGR) were carried out in accordance with ASTM E647(3)
on the 2205 and 2507 specimens17 with (water-quenched specimens) and without precipitates (untreated
specimens). The tests were carried out on compact tension specimens, C(T), with thickness of 7.5 mm and
width of 30 mm. The determination of FCGR was also performed on hydrogen pre-charged specimens. The
hydrogen charging was carried out by cathodic polarization at room temperature, in a 1N H2SO4 solution,
with a cathodic current of 0.25 A, with a current density of 10 A/cm 2 and for 1 hour. The pre-charged
specimens were labelled with the suffix –H. The fatigue cycling of the C(T) specimens for the determination

(1)NACE: National Association of Corrosion Engineer - 15835 Park Ten Pl, Houston, TX 77084, (USA).
(2)NORSOK: Standard Norway – Strandveien 18, P.O. Box2 N-1326 Lysaker Norway.
(3)ASTM International: American Society for Testing and Materials International - 100 Barr Harbor Drive, PO

Box C700 - 19428-2959 West Conshohocken (PA, USA).

©2018 by NACE International.
Requests for permission to publish this manuscript in any form, in part or in whole, must be in writing to
NACE International, Publications Division, 15835 Park Ten Place, Houston, Texas 77084.
The material presented and the views expressed in this paper are solely those of the author(s) and are not necessarily endorsed by the Association.
2
 of FCGR was carried out with a Zwick Vibrophore 250 equipped with a secondary cell load of 25 kN at room
temperature, with a frequency of the applied load of 45-50 Hz and with a ratio (R) of the applied load equal to
0.1.

The potentiodynamic polarization tests were carried out on specimens polished up to 2500 grit. These tests
were conducted at temperatures of 53.0°C and 46.0°C for the 2507 and 2205 specimens respectively with a
1M NaCl solution as electrolyte. The working electrode of the test was the DSS specimen, a saturated
calomel electrode (SCE) was used as the reference electrode and a platinum foil was used as the counter
electrode. The range of the potential was set to -0.4 V to 1.5 V (vs. SCE) and the potential rate was set to
0,005 V/s.

Table 1 lists all the specimens investigated in this paper.

Table 1: Test Specimens Identification

HEAT COOLING HYDROGEN PRE-CHARGING

SPECIMEN LABEL DSS
TREATMENT MEDIA CATHODIC POLARIZATION
2205 UNS S32205 None None No
2205A UNS S32205 1 h at 1200°C Air No
2205O UNS S32205 1 h at 1200°C Oil No
2205W UNS S32205 1 h at 1200°C Water No
2205H UNS S32205 None None Yes
2205WH UNS S32205 1 h at 1200°C Water Yes
2507 UNS S32750 None None No
2507A UNS S32750 1 h at 1200°C Air No
2507O UNS S32750 1 h at 1200°C Oil No
2507W UNS S32750 1 h at 1200°C Water No
2507H UNS S32750 None None Yes
2507WH UNS S32750 1 h at 1200°C Water Yes

RESULTS

The effects of the heat treatments on the microstructures of the 2205 and 2507 DSS are shown in Figures 1-
4. The chemical compositions of the investigated DSS are reported in Table 2.

The untreated specimens exhibited the typical microstructure of DSS, composed of austenite and ferrite (Fig.
1). In the air-cooled specimens (slowest cooling rate), shown in Fig 2, the appearance of precipitates were
observed. In the 2205 specimens, coarse precipitates were detected at the grain boundaries as carbides and
nitrides; in the 2507 specimens, the presence of coarser grain boundary precipitates were coupled with
some scattered intragranular quenched-in chromium nitrides inside the ferrite grains. A higher quenched-in
Cr2N content was observed in the oil-cooled specimens where some clouds of these precipitates were
detected (Fig. 3); in particular, a slightly higher density of Cr2N was observed in the 2507 specimen. The
water-quenched specimens (fastest cooling rate) revealed the highest quenched-in Cr2N whilst the 2205
specimen exhibited clouds of quenched-in Cr2N together with few precipitates at the grain boundaries; the
2507 specimens showed a strong precipitation of quenched-in nitrides in the form of clouds inside the ferrite
grains (Fig. 4).

An HV10 hardness characterization was carried out on each specimen. These results are reported Fig. 5a
and show an increment in the hardness of the 2507 specimens; as the nitride content is increased (increase
in cooling rate) reaching the highest value of 290 HV for the specimen 2507W; the other values for this
material are around the values measured on the untreated specimen (~270 HV). The 2205 specimens
revealed a different trend; indeed, the results were all around the value of the untreated specimen (~260
HV).

©2018 by NACE International.

Requests for permission to publish this manuscript in any form, in part or in whole, must be in writing to
NACE International, Publications Division, 15835 Park Ten Place, Houston, Texas 77084.
The material presented and the views expressed in this paper are solely those of the author(s) and are not necessarily endorsed by the Association.
3
 Fig. 5b shows the average absorbed energies obtained from the impact toughness tests at temperature of -
46°C. The values of the specimens without chromium nitrides (untreated specimens) were reached around
300 J. The lowest values observed for the air-cooled specimens, in particular the specimens 2205A,
revealed one single value below 40 J.

The pitting corrosion tests results are shown in Fig. 5c; no relevant weight loss was observed apart from the
2507W specimen that exhibited a weight loss close to 1 g/m2.
The ferrite content (Fig. 5d), was almost constant and scattered around 58% for the treated and untreated
2507 specimens and was around 61% for the 2205.

The potentiodynamic polarization tests results reported in Fig. 6 reveal that the specimens with the highest
Cr2N content (-W specimens) showed the same kind of hysteresis and signs of pitting corrosion. For the
parent metal 2507 (untreated) there was no hysteresis cycle and a presence of the oxygen evolution. The
2507A specimen showed little hysteresis and small pits whilst the 2507O specimen did not show any sign of
transpassive corrosion given the fact that 53.0°C is lower than the critical pitting temperature (CPT) of
60.0°C. For the DDS 2205 parent metal there were signs of pitting corrosion (positive hysteresis) but for the
2205A specimen there was only the passivation phase, and lastly for the 2205O specimen, one can observe
the beginning of the comparison of stable pits.

Fig. 7 shows the FCGR obtained for the specimens with the highest chromium nitride content (2205W and
2507W) and without precipitates (2205 and 2507). These are reported together with the results obtained
from the same kind of specimens after hydrogen pre-charging (2205H, 2507H, 2205WH and 2507WH), and
the curves are superimposed in this graph. It can be observed that at low fatigue crack growth rate values,
da/dN, the wave for the specimens with Cr2N shifted to higher values of the stress intensity factor range,
K,
than those without Cr2N. However, at higher da/dN, the curves for the specimens with Cr2N are steeper,
hence they have faster crack growth rates.

In Table 4 the data obtained from the FCGR tests are shown together. From a general point of view, the
DSS 2205 and 2507 appeared very similar in the untreated condition. Indeed, they exhibited values of C
around 10-11 and values of the slope m close to 2.7. The specimens with Cr2N (2205W and 2507W) showed
the same behaviour, otherwise a shift to higher values of the threshold stress intensity factor range,
Kth, and
an increase of m compared to the data obtained from the untreated specimens (
Kth from 7.42 to 17.23
MPam0.5 and from 9.02 to 10.05 MPam0.5 for the 2205 and 2507 specimens respectively; m from 2.78 to 3.34
and from 2.67 to 4.33 for the 2205 and 2507 specimens respectively). The same differences between
specimens with or without Cr2N were observed on the hydrogen pre-charged specimens (
Kth from 9.88 to
14.88 MPam0.5 and from 7.94 to 10.76 MPam0.5 for the 2205 and 2507 specimens respectively; m from 2.43
to 3.10 and from 2.91 to 3.01 for the 2205 and 2507 specimens respectively).

Table 2: Chemical composition (% weight)

ELEMENT 2507 2205

C 0.020 0.028
Si 0.307 0.457
Mn 0.812 1.340
P 0.0264 0.0271
S 0.0011 0.0005
Cr 24.07 22.77
Mo 3.229 2.862
Ni 6.49 5.14
N 0.3130 0.1919
Cu 0.184 0.133
W 0.026 0.044
Fe balance balance

©2018 by NACE International.

Requests for permission to publish this manuscript in any form, in part or in whole, must be in writing to
NACE International, Publications Division, 15835 Park Ten Place, Houston, Texas 77084.
The material presented and the views expressed in this paper are solely those of the author(s) and are not necessarily endorsed by the Association.
4
 Fig. 1: Untreated specimens, typical DSS microstructures composed of austenite and ferrite.

Fig. 2: Air-cooled specimens; grain boundary precipitates in the 2205 specimen; presence of some
quenched-in nitrides (inside the ferrite grains) and coarse grain boundary precipitates in the
2507 specimen.

Fig. 3: Oil-cooled specimens; clouds of quenched-in nitrides inside the ferrite grains and grain
boundary precipitates in both specimens; slightly higher content of quenched-in
chromium nitrides in the 2507 specimen.

©2018 by NACE International.

Requests for permission to publish this manuscript in any form, in part or in whole, must be in writing to
NACE International, Publications Division, 15835 Park Ten Place, Houston, Texas 77084.
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5
 Fig. 4: Water-quenched specimens; clouds of quenched-in nitrides inside the ferrite grains and grain
boundary precipitates in the 2205 specimen; heavy precipitation of chromium nitrides in the
ferrite grains in the 2507 specimen.

Fig. 5: (a) and (b) HV10 Vickers hardness indentation results and average absorbed energies at T=-
46°C respectively; the error bars indicate the maximum and the minimum values recorded
for each specimen. (c) Pitting corrosion test results. (d) Ferrite contents in percentage, the
error bars indicate an error of ± 1.5%.

©2018 by NACE International.

Requests for permission to publish this manuscript in any form, in part or in whole, must be in writing to
NACE International, Publications Division, 15835 Park Ten Place, Houston, Texas 77084.
The material presented and the views expressed in this paper are solely those of the author(s) and are not necessarily endorsed by the Association.
6
 Table 3: Summary table for the data shown in Figures 5-6 and referred, for each specimen, to the
microstructures’ comments of the Figures 1-4; the CPT values for the untreated
specimens were calculated from their chemical analyses shown in Table 2.

AVERAGE
WEIGHT FERRITE
ABSORBED CPT
SPECIMEN HV10 LOSS CONTENT MICORSTRUCTURE
ENERGY AT T = [°C]
[g/m2] [%]
-50°C [J]
2205 260 373 - 58 46.3 Austenite and ferrite
Chromium nitrides and carbides at grain
2205A 258 60 0.0287 60 46.0
boundaries
QUENCHED-IN chromium nitrides inside
2205O 260 189 0.0000 63 44.0 the ferrite grains and precipitation at grain
boundaries.
QUENCHED-IN chromium nitrides inside
2205W 256 169 0.0000 62 42.5 the ferrite grains and precipitation at grain
boundaries.
2507 267 295 - 57 55.7 Austenite and ferrite
Some QUENCHED-IN chromium nitrides
2507A 262 188 0.1320 58 54.5 inside the ferrite grains and precipitation at
grain boundaries.
QUENCHED-IN chromium nitrides inside
2507O 274 281 0.0989 60 60.0 the ferrite grains and precipitation at grain
boundaries.
Heavy precipitation of QUENCHED-IN
2507W 290 229 0.9399 58 54.5
chromium nitrides in the ferrite grains


 

                 

 

 
 
 
 

 

 

 
 
 
    
      
     

    
 
  

    

 

Fig. 6: Potentiodynamic polarization test results.

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7
 1.0E-05

1.0E-06

1.0E-07

da/dN [m/cycle]

2205
1.0E-08 2205W
2205H
2205WH
2507
1.0E-09
2507W
2507H
2507WH

1.0E-10

0
10

20

30

40

50

60

70
80
90
10
0.5
K [MPam ]

Fig. 7: FCGR (da/dN) vs. ΔK results.

Table 4: Results corresponding to the data shown in Fig. 7

SPECIMEN C m
Kth [MPam0.5]

2205 9.13E-12 2.78 7.42
2205W 7.87E-13 3.34 17.23
2205H 2.89E-11 2.43 9.88
2205WH 2.09E-12 3.10 14.88
2507 1.24E-11 2.67 9.02
2507W 3.05E-14 4.33 10.05
2507H 5.00E-12 2.91 7.94
2507WH 3.07E-12 3.01 10.76

DISCUSSION

The first conclusion that can be drawn from the results is that increasing the cooling rate, the precipitated
intragranular quenched-in Cr2N content is increased too. The effect of the cooling rate acts on the type of
compound that precipitates. In particular, in the specimens submitted to the slowest cooling rate (air-cooled
specimens) the presence of coarser precipitation at the grain boundaries was observed, probably carbides
and nitrides. These compounds diminished in the specimens cooled at higher cooling rates to leave space to
the quenched-in Cr2N. The specimens with the highest quenched-in Cr2N content were the water-quenched
2205W and 2507W.

The presence of quenched-in Cr2N in DSS, especially for the highest content, led to an increase in hardness
of the 2507 DSS and to a reduction in impact toughness of about 50% in the 2205 DSS. However, these
values are in compliance with the limit suggested by NORSOK for DSS11, respectively below 310 HV and
above 40 J. From a general point of view the treated specimens exhibited lower impact toughness values
than the untreated. Among the treated specimens, the minimum values were recorded for the –A specimens;
in particular, a single value below the 40 J limit was observed in the 2205A specimen. However, the 2507A
specimen exhibited an impact toughness well above this limit and near to the values obtained for the 2507O
©2018 by NACE International.
Requests for permission to publish this manuscript in any form, in part or in whole, must be in writing to
NACE International, Publications Division, 15835 Park Ten Place, Houston, Texas 77084.
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8
 and 2507W specimens. This behaviour can be explained by attributing the decrease in toughness to the
coarser precipitates detected in the microstructure of the 2205A and 2507A specimens, characterized by
slow cooling rates.

The pitting corrosion tests did not reveal any relevant weight loss apart from the value of around 1 g/m2 for
the 2507W specimen. Nevertheless, this value is below the limit of 4 g/m2 suggested by NORSOK for DSS10.
The results of the potentiodynamic polarization tests can be seen as consistent with the CPT test, given that
the 2507O specimen did not show any signs of transpassive corrosion, and that this is due to the
temperature used (53.0°C) being lower than the temperature needed to form the first stable pit (60.0°C); a
similar observation can be made for the 2205A that needed a slightly higher temperature than its CPT
(46.0°C). The 2205W and 2507W specimens show a positive hysteresis cycle which means an inherent
difficulty for the metal in pitting re-passivation; this can be the result of the quenched-in Cr2N that was
observed in the microstructure.

The FCGR tests in air revealed a shift to higher values of the
Kth for the specimens with high content of
quenched-in Cr2N. This means that in a DSS with quenched-in Cr2N, a higher minimum stress intensity
factor is required to propagate a crack than in a DSS without Cr2N. However, when a crack starts
propagating, the presence of Cr2N promotes the crack growth to faster rates than in a DSS without Cr2N.
No relevant differences are noticeable comparing the results for the hydrogen pre-charged specimens to
those that are not pre-charged.

CONCLUSIONS

Different Oil&Gas standards (NACE, NORSOK 10,11) require specific quantitative limits for general
intermetallic content (e.g. 0.5-1%) including nitrides. During material and welding qualification, a detailed
quantification of clouds of intragranular quenched-in nitrides could be tricky and time consuming. Therefore,
in this paper, specimens with forced quenched-in nitride precipitation were created to investigate in-depth the
effect of Cr2N on the engineering properties of DSS. Lastly, on the basis of the results obtained, the
concluding remarks are listed as follows:

 The corrosion resistance and toughness (impact tests) properties of the specimens with the
highest quenched-in Cr2N content were slightly affected but remained in compliance with the
most commonly applied standard requirements.

 The minimum impact toughness values were observed on the specimens without quenched-in
Cr2N and affected by the presence of coarser precipitates at grain boundaries.

 A slight increase in hardness was observed increasing the quenched-in Cr2N content, however it
was below the typical maximum limit for sour service (310HV)

 The potentiodynamic polarization test confirmed that Cr2N has some effects on DSS,
furthermore, the specimens with the higher Cr2N content showed a very positive hysteresis
cycle.

 The FCGR tests in air revealed a slight negative effect of quenched-in Cr2N; in particular, it was
observed that in 2507 DSS the presence of quenched-in Cr2N increased the fatigue crack growth
rate; the same effect was observed in 2205 DSS.

 The effect of hydrogen charging on the FCGR was the same on the specimens with or without
quenched-in Cr2N; no relevant effects were observed.

 Quenched-in Cr2N precipitation can be considered as not being detrimental to the engineering
properties of the DSS 2205 and 2507, taking into account the more common standard
requirements applied in Oil & Gas.

 Detailed quantification of quenched-in Cr2N can be considered as useless.

 Visual comparison between reference micrographic images (to be adopted by standards) can be
proposed as a more practical approach in QA/QC procedure for DSS.

©2018 by NACE International.

Requests for permission to publish this manuscript in any form, in part or in whole, must be in writing to
NACE International, Publications Division, 15835 Park Ten Place, Houston, Texas 77084.
The material presented and the views expressed in this paper are solely those of the author(s) and are not necessarily endorsed by the Association.
9
 FUTURE WORK

Further FCGR tests in a corrosive environment and under cathodic polarization will be carried out as future
work together with Stress Corrosion Test and Sulphide Stress Corrosion Test.

ACKNOWLEDGEMENTS

The authors wish to thank Dr. Elin M. Westin for her interest and support in this paper.

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©2018 by NACE International.

Requests for permission to publish this manuscript in any form, in part or in whole, must be in writing to
NACE International, Publications Division, 15835 Park Ten Place, Houston, Texas 77084.
The material presented and the views expressed in this paper are solely those of the author(s) and are not necessarily endorsed by the Association.
10