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Article history: Three weldments with the nickel contents 1.3, 4.9 and 6.0 wt% were made from 30 mm LDX 2101s
Received 21 October 2013 plates. The weldments were subjected to tensile, impact and fracture toughness testing. The aim was to
Received in revised form evaluate the susceptibility for brittle failure in the weld metal at sub-zero temperatures (1C). The amount
29 January 2014
of ferrite was higher for the 1.3 wt% nickel weldment compared to the other two which had similar phase
Accepted 30 January 2014
Available online 6 February 2014
composition and mean free ferrite distance. The result from the tensile testing showed that for the
weldment with the highest nickel content the ductility remained unchanged with decreasing tempera-
Keywords: ture while the other two weldments became less ductile with decreasing temperature. J-integral based
Duplex stainless steel fracture toughness testing showed a significant difference in the susceptibility for brittle failure with
Weld metal
higher values for the weldment with 6 wt% nickel than for the others with lower nickel content.
Impact toughness
& 2014 Elsevier B.V. All rights reserved.
Fracture toughness
Nickel
http://dx.doi.org/10.1016/j.msea.2014.01.093
0921-5093 & 2014 Elsevier B.V. All rights reserved.
50 J. Pilhagen, R. Sandström / Materials Science & Engineering A 602 (2014) 49–57
Table 1
Chemical composition (wt%) of the plate and filler metals. Measured with X-ray fluorescence and combustion analysis.
C Si Mn P S Cr Ni Mo N
LDX 2101s 0.028 0.65 4.95 0.024 0.001 21.5 1.59 0.26 0.22
Autogenous experimental filler, Ø 2.4 mm 0.021 0.74 4.95 0.017 0.001 20.62 1.28 0.10 0.24
Standard commercial filler 23 7 NL, Ø 1.2 mm 0.020 0.50 0.71 0.018 0 23.13 7.30 0.25 0.12
Table 2
Welding parameters for the three weldments.
Root gap, mm Land, mm Groove angle, deg Heat input, kJ/mm Current, A Voltage, V Welding speed, cm/min
n
Numbers in parenthesis are for the root when different filler metals or welding methods were used.
Table 3
EDS analysis of the weldments showing the average value. Min–max values in parentheses. Nitrogen and oxygen content measured by combustion analysis.
Fe, wt% Cr, wt% Mn, wt% Ni, wt% N, wt% O, ppm
1.3 Ni 69.56 (67.84–71.94) 22.01 (21.33–23.04) 4.01 (3.53–4.55) 1.34 (1.01–1.71) 0.184 371
5 Ni 69.20 (68.27–70.17) 22.06 (21.27–22.84) 3.04 (2.00–3.73) 4.93 (3.87–5.92) 0.178 348
6 Ni 66.89 (64.78–69.35) 22.92 (21.76–24.14) 1.47 (0.78–2.31) 6.02 (5.30–6.63) 0.137 294
Table 4 For the 1.3 Ni and 5 Ni weldment the nitrogen was however lower
Phase composition of ferrite in the weldments. Automatic image analysis based on in the weldment than in the base metal which can possibly be
ASTM E1245 [11]. associated to outgassing of nitrogen during welding.
The phase composition of the weldments can be found in
α-content, vol% STDEV 95% Confidence interval
Table 4. The 5 Ni and 6 Ni weldments had similar phase composi-
1.3 Ni 79.6 3 1.2 tion but the 1.3 Ni had clearly higher ferrite content. The ferrite
5 Ni 57.4 7.9 3.3 content at the root was higher, 62% and 63% for the 5 Ni and
6 Ni 59.3 7.7 3.6 6 Ni respectively, compared to the average values in Table 4. For
the 1.3 Ni weldment the ferrite content was lower, 72% at the
root weld compared to the average values in Table 4. The likely
explanation was that for the 5 and 6 Ni weldments the nickel
The welding procedures for these weldments were: content was reduced at the root due to dilution with the base
metal. The lower energy input in the MIG welding also contributed
Submerged arc welding (SAW) with autogenous experimental to the higher ferrite content in the root for the 6 Ni weldment. For
filler. The low nickel content of this autogenous experimental the 1.3 Ni weldment the nickel content was instead increased due
filler will enable studies of brittle fracture. to dilution (lower nickel content in the filler metal compared to
SAW with standard commercial filler for the two root beads the base metal).
where the dilution is high. The remaining 16 beads were In Fig. 1 representative light optical microscope (LOM) photos
submerged arc welded with the autogenous experimental filler of the microstructure for the three different weldments are shown.
and nickel powder additions of 2.5–4.9 g/bead. This configura- The microstructure consists of intergranular (grain boundary),
tion enables comparison with the previous low nickel weld. intragranular and Widmanstätten austenite in a ferrite matrix.
Metal inert gas (MIG) welding of the first 7 beads and SAW for By observing the microstructure in LOM, the 1.3 Ni weldment
the remaining 11 beads. The standard commercial filler metal seemed to have less degree of Widmanstätten austenite compared
23 7 NL was used for both methods. This configuration serves to the 5 Ni and 6 Ni weldments. The 5 Ni and 6 Ni weldments were
as a reference weld. indistinguishable from each other. No intermetallic phases were
observed.
For the SAW welding the flux material used had the following For duplex stainless base metals with its highly elongated
chemical composition (wt%): 7 SiO2, 50 CaF2, 36 Al2O3, 3 Cr. microstructure the austenite lamellar spacing have been found
Result from energy-dispersive X-ray spectroscopy (EDS) across to influence the impact toughness [12] and used for regression
the weldments (through-thickness) is shown in Table 3. Small analysis of yield and tensile strength [13,14]. For the weld metal
samples were also cut out from the weld metal of the tested the microstructure was more complex so the mean free ferrite
specimens for combustion analysis of the nitrogen and oxygen distance was used to characterize the weld metal. Line intercept
content. The main differences in chemical composition were in the counting with LOM at 100 magnification on polished and etched
manganese, nickel and nitrogen content. The weldments are in samples of the weldments revealed that the 5 and 6 Ni weldments
this paper named 1.3 Ni, 5 Ni and 6 Ni. had similar mean free ferrite distance, see Table 5. The much larger
For the 6 Ni weldment the manganese content and nitrogen mean free ferrite distance for the 1.3 Ni weldments was explained
content was likely increased due to dilution with the base metal. by the higher ferrite phase content.
J. Pilhagen, R. Sandström / Materials Science & Engineering A 602 (2014) 49–57 51
Table 5
LOM measurement of the mean free ferrite distance.
Table 6
Straightness of the pre-crack fronts.
1.3 Ni þ20 –
1.3 Ni 1 –
1.3 Ni 21 –
1.3 Ni 41 –
5 Ni þ20 Accepted, 9(2–8) pointa
5 Ni 1 Accepted, 9(2–8) point
5 Ni 20 Accepted, 9 pointb
5 Ni 40 Accepted, 9 point
6 Ni þ20 Accepted, 9 point
6 Ni 1 Accepted, 9(2–8) point
6 Ni 21 Accepted, 9 point
6 Ni 40 No local compressionc
6 Ni 50 Accepted, 9 point
6 Ni 60 Accepted, 9 point
a
Pre-crack front measured as stated in ASTM E 1820 points No. 1 and 9 were
ignored.
b
Pre-crack front measured as stated in ASTM E 1820.
c
Pre-crack front as in Fig. 2a.
4. Results
to fatigue precracking and side grooving. The procedure followed
the one described in BS7448 [15]. 4.1. Tensile tests
The result from the local compression can be seen in Fig. 2. For
the as-received specimen (without local compression) most of the The yield and tensile strength of the weldments can be found in
fatigue crack growth occurred at the sides and hardly at all in the Fig. 3. It was evident that the yield and tensile strength increases
middle of the specimen. For the local compressed specimens the with decreasing temperature. The 1.3 Ni weldment had the lowest
fatigue crack growth took place more evenly across the cross mechanical strength and the 5 Ni weldment the highest.
section. The fracture behavior of the three weldments at room tem-
The target for the total plastic deformation was 0.8%. The perature was ductile failure after necking with some local regions
resulting value was between 0.63% and 1%. As can be seen in (circular with a diameter of 1 mm) of initiated transcrystalline
Fig. 2b the fatigue crack front has grown more in the middle of the cleavage fractures. In the center of each local cleavage region a gas
specimen, giving a slightly thumbnail shape which might indicate pore was found. The failure was likely to occur when cleavage
that the plastic deformation was a bit too high. fracture was initiated from this gas pore. This reduced the bearing
The measurement of the length of the fatigue pre-crack was capacity of the specimen causing specimen failure. At 0 1C the
measured from nine equally spaced points along the pre-crack 1.3 Ni weldment failed by complete cleavage fracture prior to
front [ASTM 1820]. The point Nos. 1 and 9 were measured 0.005 necking. With further reduced temperature the elongation to
times the specimen width from the side-groove edge. The average fracture decreased as shown in Table 7. The 5 and 6 Ni specimens
of the two values at the edges was averaged with the average of had the same type of failure event at lower temperatures as at
the remaining values. The maximum deviation from this average room temperature. For the 5 Ni specimens the elongation to
pre-crack length is 1.5 mm for a SE(B) specimen with 30 mm fracture decreased with reducing temperature.
thickness [ASTM 1820].
In Table 6 the straightness of the pre-crack front for the 4.2. Impact toughness
specimens is shown. For the 1.3 Ni specimens the fatigue pre-
cracking led to an irregular pre-crack front. Some regions were less The Charpy V impact toughness of the weldments is shown in
affected by the fatigue precracking than other and some regions Fig. 4. The 1.3 Ni weldments had the lowest impact toughness
inside the pre-crack region were unaffected by the fatigue pre- while the 6 Ni weldments had the highest one. The 1.3 Ni was
cracking. No meaningful measurement of the pre-crack length brittle at all test temperatures with clearly visible transcrystalline
could therefore be obtained. For the 5 Ni specimens at þ20 and at cleavage fracture facets.
1 1C the fatigue crack growth was less at the edges of the For the 5 Ni specimen at room temperature with the highest
specimens. The result was a thumbnail shaped pre-crack front. impact toughness, the fracture surface was dominated by shear
The maximum difference between the two near surface points and lips and ductile failure. Small local regions of arrested cleavage
the average crack length exceeded 1.5 mm and the straightness of fractures were also visible. The other two specimens at room
J. Pilhagen, R. Sandström / Materials Science & Engineering A 602 (2014) 49–57 53
1000 Table 8
1.3 Ni Results from the fracture toughness testing.
950 5 Ni
900 6 Ni T, 1C Jc, kN/m JIc, kN/m Test event
Rp0.2
850 Rm 1.3 Ni þ 20 6.3 Na Unstable failure
1.3 Ni 1 8.3 Na Unstable failure
Stress [MPa]
140 growth (on average 2.84 mm) prior to the unstable failure so valid
120 initiation fracture toughness could be obtained. At 20 1C the stable
crack growth decreased to about 100 μm prior to the unstable failure.
100 The result from the fracture toughness testing follows the same
80 ranking as for the impact toughness result, see Table 8 and Fig. 5.
The fracture toughness value for the point of fracture instability
60
was defined by the Jc criteria in ASTM 1820-06 [16]. The ductile
40 initiation fracture toughness, JIc, was evaluated according to the
normalization data reduction method in ASTM 1820-06 [16].
20
found for these specimens. Only for one fracture toughness speci- was larger for the 1.3 Ni weldments than for the other weldments,
men a gas pore was observed close to the crack-tip, see Fig. 7a. recall Table 5.
As was evident from the SEM photo, cleavage fracture occurred The chemical composition of the weldments mainly differs for
prior to the gas pore and ductile fracture was observed almost three elements, manganese, nickel and nitrogen, recall Table 3.
around the entire pore. One can conclude that the cleavage fracture Previous regression analysis of the yield and tensile strength of
initiation in toughness specimens was not caused by gas pores. base material of duplex and austenitic stainless steels includes a
contribution from the ferrite phase, the lamellar spacing and the
manganese, nickel and nitrogen content [13,14]. If one assumes
that the lamellar spacing reflects the value of the ferrite mean free
5. Discussion
path, the results from the tensile testing in Fig. 3, can be under-
stood: the 1.3 Ni specimens have higher ferrite content and
5.1. Tensile properties
a higher mean free ferrite path, which give a reduction in yield
strength compared to the other two types of weldments. This
As shown in Table 4, the phase composition was similar for the
reduction was somewhat offset by the higher manganese and
5 Ni and 6 Ni weldments while the 1.3 Ni weldment had much
higher ferrite content. As a consequence the mean free ferrite path
700
6 Ni
5 Ni
600
1.3 Ni
500
400
J [kN/m]
300
200
100
0
−60 −40 −20 0 20
Temperature [°C]
Fig. 5. Fracture toughness of the weldments. The data points are from Table 8. Fig. 7. Gas pore close to the crack-tip in the 5 Ni specimen tested at 40 1C.
Fig. 6. SEM examination of various fracture surfaces from the fracture toughness tested specimens. (a) Cleavage fracture initiation causing pop-in during precracking, 1.3 Ni
specimens at þ 20 1C, (b) microvoid coalescence fracture, 6 Ni specimen at þ20 1C, (c) fracture initiation at 21 1C for the 6 Ni specimen and (d) fracture initiation at 40 1C
for the 5 Ni specimen.
J. Pilhagen, R. Sandström / Materials Science & Engineering A 602 (2014) 49–57 55
1050 0.2
1000 0.18
0.16
950
True tensile stress [MPa]
0.14
εtrue,necking [m/m]
900
0.12
850
0.1
800
0.08
750 0.06
700 0.04
1.3 Ni
1.3 Ni
650 0.02 5 Ni
5 Ni
6 Ni
6 Ni
0
600 −50 −40 −30 −20 −10 0 10 20 30
−40 −30 −20 −10 0 10 20
Temperature [°C] Temperature [°C]
Fig. 9. True strain to necking at necking or failure before necking for the tensile
Fig. 8. True tensile stress at necking or failure before necking of the tensile
specimens.
specimens.
nitrogen content in the 1.3 Ni weldment. With the same reasoning the reduced ductility for the 5 Ni weldment with decreasing
the 5 Ni weldment have higher yield strength than the 6 Ni temperature would then be that the necking (point of instability)
weldment due to the higher manganese and nitrogen content. The occurs at lower strains due to change in dislocation behavior. For
tensile strength was further increased compared to the 6 Ni the 6 Ni weldment this change in dislocation behavior occurs at
weldment due to the lower nickel content in agreement with lower temperatures than tested and therefore the strain to necking
the observations. A similar argument for tensile specimens can be was unchanged.
found in [20] for some experimental duplex stainless alloys with The difference in fracture behavior during fracture toughness
different phase composition, grain sizes, manganese and nickel testing between the 5 Ni and 6 Ni weldments with decreasing
contents. The lower tensile strength for the 1.3 Ni weldment can temperature was that the 5 Ni specimens failed catastrophically at
also partially be explained by the fact that this weldment only a lower force. Both weldments exceeded 90 kN at room tempera-
reached necking at room temperature. One should note that the ture and with reduced temperature the 5 Ni failed at 63 kN at 0 1C,
published regression analyses were made from specimens tested 57 kN at 20 1C and 38 kN at 40 1C. The 6 Ni weldment
at room temperature so any temperature dependence of the yield remained at 90 kN until 40 1C where it failed at 71 kN. The
and tensile strength was not incorporated. crack-tip blunting and the region of ductile fracture prior to
cleavage fracture decreased greatly with decreasing temperature
5.2. The influence of nickel for the 5 Ni weldment.
For impact toughness and fracture toughness specimens, the
The results of the tensile tests, Fig. 3, show a similar engineer- material volume that was affected by the loading, the process
ing stress evolution (yield and tensile strength) with decreasing zone, was much smaller compared to the entire volume of the
temperature for the three different weldments. If one instead tensile specimen. The results were therefore largely dependent on
evaluates the tensile testing by using true stress and true strain the notch/crack-tip location in relation to cleavage fracture initia-
under the assumption of constant volume, the three weldments tion sites (inclusion, carbides, nitrides, intermetallic phases, etc.)
behavior with decreasing temperature were different. Fig. 8 shows in the material. This gives high scatter for impact and fracture
the true stress at necking for the 5 Ni and 6 Ni tensile specimens toughness when tested in the ductile to brittle transition region.
and the true stress at necking at room temperature and the true This can be seen from the impact toughness testing where three
stress at failure at the other testing temperatures for the 1.3 Ni specimens at each temperature were tested, Fig. 4. For the fracture
weldment. The 1.3 Ni and 5 Ni specimens have a fairly tempera- toughness testing only one specimen per temperature was tested
ture independent true stress to necking/failure while the 6 Ni so the scatter was unknown. The results from the impact and
specimens have a true stress to necking that increases with tensile testing indicate, however, that the difference in fracture
decreasing temperature. This difference in behavior with decreas- toughness between the 5 Ni and 6 Ni reflects the increased
ing temperature was also clearly seen for the true strain to resistance to cleavage fracture initiation in the 6 Ni weldment.
necking, see Fig. 9. The 1.3 Ni and 5 Ni weldments loose ductility The two weldments 5 Ni and 6 Ni had similar phase composi-
with decreasing temperature while for the 6 Ni weldment the tion and microstructure characteristics, recall Tables 4 and 5. The
ductility was approximately unchanged for the tested temperature chemical composition differs mainly in the nitrogen and manga-
interval. nese content. However, for duplex stainless steel weld metals the
From impact toughness testing of low carbon alloys with element partitioning is less expressed than for the base metal.
varying nickel content it has been shown that nickel increases Normally during welding the cooling of the weld metal is too rapid
the cleavage stress and shifts the ductile-to brittle transition for the diffusion of the substitutional solute elements (Cr, Mo, Mn
temperature to lower temperatures [6,7]. One explanation given and Ni) to play a significant role in the austenite formation [21,22].
is that nickel increases the ability for dislocations to cross-slip in Instead the austenite formation is governed by the diffusion of the
the ferritic phase [7] which would decrease the local stress from interstitial elements carbon and in particular nitrogen [21,22]. The
dislocation pile-ups around cleavage fracture initiation sites. This nitrogen content in the ferrite was thereby likely to be similar
increased ability for cross-slip due to nickel has been observed by between the two weldments. To the authors' knowledge, manga-
Jolley [6]. The high cleavage fracture susceptibility for the 1.3 Ni nese has no inherent detrimental effects on the ferrites suscept-
weldment can be explained by the high ferrite content with large ibility for cleavage fracture except for the increase in yield
mean free ferrite path and low nickel content. An explanation for strength. Reduced impact toughness with increased manganese
56 J. Pilhagen, R. Sandström / Materials Science & Engineering A 602 (2014) 49–57
Table 9
Microstructure properties and nickel content for various duplex stainless steel weld metals. Standard deviation in parenthesis.
α Phase contenta, % 63.9 ( 7 2.7) 44.0 ( 79) 45 ( 76) 57.4 ( 7 7.9) 59.3 ( 7 7.7)
γ Phase contenta, % 36.1 (7 2.7) 56.0 ( 7 9) 55 ( 76) 42.6 ( 7 7.9) 40.7 ( 7 7.7)
Average mean free distance, weld roota, μm – – 16.6 ( 7 3.9) 20.5 ( 7 4.0) 15.9 ( 7 2.4)
Average mean free distance, welda, μm 22.9 ( 7 3.4) – – 11.1 ( 7 1.2) 11.6 ( 7 1.7)
Average Ni content in weldb, wt% 7.7 ( 7 0.2) – 8.2 (7 0.6) 5 6.1 ( 7 0.4)
Average Ni content in αc, wt% 7.4 ( 7 0.3) – 8.3 (7 0.4) – 6.2 ( 7 0.2)
Average Ni content in γc, wt% 7.9 ( 7 0.4) – 8.2 (7 0.5) – 6.1 ( 7 0.2)
a
Measured from etched samples by LOM.
b
Area analyses on polished samples by EDS.
c
Average spot analyze, 7 measured spots for each phase at random locations.
200
2205 WM, K−joint the filler metal usually, the nickel content in the weld metal can
180 2304 WM, X−joint decrease with decreasing fracture toughness as a result [25]. The
2101 WM, X−joint
160 lean duplex stainless steel with its low nickel content is more
6 Ni, X−joint
140 5 Ni, X−joint susceptible to this than DSS grades with higher nickel content.
120
JC [kN/m]
[6] W. Jolley, Trans. Metall. Soc. AIME 242 (1968) 306–314. [18] O.L. Towers, M.G. Dawes, Welding institute research on the fatigue pre-cracking
[7] S. Floreen, H.W. Hayden, T.M. Devine, Metall. Trans. 2 (1971) 1403–1406. of fracture toughness specimens, Elastic–Plastic Fracture Test Methods: The
[8] R.N. Gunn, Duplex Stainless Steels – Microstructure, Properties and Applica- Users Experience, ASTM STP 856, April 1985, Ann Arbor.
tions, Woodhead Publishing Ltd., Abington Hall, 2003(pp. 122). [19] M.G. Dawes, H.G. Pisarski, S.J. Squirrell, Fracture Mechanics Tests on Welded
[9] H. Sieurin, R. Sandström, E.M. Westin, Metall. Mater. Trans. A 37A (2006) Joints, in: J.D. Landes, A. Saxena, J.G. Merkle (Eds.), Nonlinear Fracture
2975–2981. Mechanics: Vol. II–Elastic – Plastic Fracture, ASTM STP 995, American Society
[10] H. Sieurin, E.M. Westin, M. Liljas, R. Sandström, Weld. World 53 (3–4) (2009), for Testing and Materials, Philadelphia, 1989, pp. 191–213.
R24–R33. [20] S.M. Wessman, S. Hertzman, R. Pettersson, R. Lagneborg, M. Liljas, Mater. Sci.
[11] ASTM E 1245: Standard Practice for Determining the Inclusion or Second- Technol. 24 (3) (2008) 348–355.
Phase Constituent Content of Metals by Automatic Image Analysis, vol. 03.01. [21] R.N. Gunn, Duplex Stainless Steels – Microstructure, Properties and Applica-
[12] E.M. Westin, B. Brolund, S. Hertzman, Steel Res. Int. 6 (2008) 473–481. tions, Woodhead Publishing Ltd., Abington Hall, 2003(pp. 120).
[13] H. Sieurin, J. Zander, R. Sandström, Mater. Sci. Eng. A 415 (2006) 66–71. [22] E.M. Westin, S. Hertzman, Element distribution in lean duplex stainless steel
[14] R.N. Gunn, Duplex Stainless Steels – Microstructure, Properties and Applica- welds, In: E.M. Westin, Microstructure and Properties of Welds in the Lean
tions, Woodhead Publishing Ltd., Abington Hall, 2003(pp. 58). Duplex Stainless Steel LDX 2101, Doctoral Thesis in Material Science, 2010,
[15] BS7448 Part 2: Method for Determination of KIc Critical CTOD and Critical J KTH Royal Institute of Technology, Stockholm, Sweden.
Values of Welds in Metallic Materials, seventh draft (revised), 1996. [23] E. Keehan, L. Karlsson, H.-O. Andrén, L.-E. Svensson, Weld. J. 85 (10) (2006)
[16] ASTM E 1820-06: Standard Test Method for Measurement of Fracture Tough- 218–224.
ness, vol. 03.01. [24] H. Sieurin, R. Sandström, Eng. Fract. Mech. 73 (2006) 377–390.
[17] ASTM E 1921-05: Standard Test Method for Determination of Reference [25] L. Karlsson, H. Arcini, E.-L. Bergquist, J. Weidow, J. Börjesson, Weld. World 54
Temperature, T0, for Ferritic Steels in the Transition Range, vol. 03.01. (11–12) (2010) 350–359.