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Materials Science and Engineering A 528 (2011) 5566–5575

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Materials Science and Engineering A


journal homepage: www.elsevier.com/locate/msea

In situ study of structural integrity of low transformation temperature


(LTT)-welds
J. Altenkirch a,∗ , J. Gibmeier a , A. Kromm b , Th. Kannengiesser b , Th. Nitschke-Pagel c , M. Hofmann d
a
Karlsruhe Institute of Technology (KIT), Institute of Applied Materials (IAM), Campus South, Kaiserstr. 12, 76131 Karlsruhe, Germany
b
BAM Federal Institute for Materials Research and Testing, Unter den Eichen 87, 12205 Berlin, Germany
c
Institute for Joining and Welding, TU Braunschweig, Langer Kamp 8, 38106 Braunschweig, Germany
d
FRMII, TU-Munich, Lichtenbergstr. 1, 85747 Garching, Germany

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

Article history: We discuss the stability of weld residual strain under static and quasi cyclic transverse tensile loading in
Received 26 January 2011 the elastic and elastic–plastic region. The test welds were joined with low transformation temperature
Received in revised form 22 March 2011 weld filler materials with 10 wt% Cr and varying Ni-content from 8 to 12 wt%. Using neutron diffraction
Accepted 23 March 2011
the residual lattice strain in the martensitic ␣ - and austenitic ␥-phase in the fusion zone as well as the
Available online 29 March 2011
ferritic ␣-phase in the heat affected zone and base metal as (1) induced by welding, (2) superimposed by
stepwise tensile loading and (3) after unloading was measured. The amount of retained austenite in the
Keywords:
fusion zone increases with increasing Ni-content, but it decreases with increasing load level due to stress
Low transformation temperature
Residual stress
induced martensite formation. In the as-welded condition the transverse macroscopic residual lattice
Neutron diffraction strain was found to be in low compression in the fusion zone in each weld, while the heat affected zone
was in tension. Local plastic deformation of the ␥-phase as a result of yielding during tensile loading in
combination with the change in phase fraction resulted in increased macroscopic compression in the
fusion zone. The reduced yield strength in the heat affected zone resulted in plastic deformation and a
considerable shift into compression. Comparison with the cross weld distribution of the hardness and
FWHM of the neutron diffraction interference lines supported the assumption of plastic deformation of
the ␥- and ␣-phase in the fusion and heat affected zone, respectively, while the ␣ -phase in the fusion
zone was stressed within the elastic regime only. Microstructural observations as well as measurement
of the local ␥-phase fraction by means of laboratory X-ray diffraction in the fusion zone strengthen these
observations.
© 2011 Elsevier B.V. All rights reserved.

1. Introduction ence the RS field through the weld depth (e.g. thermal treatments).
However in welding practice post-weld treatments are relatively
Tensile residual stresses (RS) as generated in welds are of major unpopular as they are time consuming and cost intensive or even
concern for structural integrity assessment in industrial compo- rather impractical due to the size and design of large or inaccessible
nents [1,2]. In-service tensile loads superimpose with weld RS and components, such as pressure pipes or ship building components.
in case these are tensile this results in a reduction of the maxi- Therefore preferable solutions should be concentrated on the pro-
mum bearable load of the component. Further tensile RS impair duction process and that is to say that it would be favourable to
the fatigue and stress corrosion behaviour of the component [2–4]. enable the generation of beneficial RS conditions directly during
It is therefore desired to reduce tensile welding RS or even to intro- the welding process.
duce compressive RS to the weld. Several mechanical as well as In steel the austenite (␥) to martensite (␣ ) phase transfor-
thermal in situ and post-weld treatment methods and combina- mation, which is accompanied by significant shear and volume
tions of these methods exist for application during or after welding strains, influences the local RS field. Therefore, controlling the ␥–␣ -
in order to reduce detrimental tensile or to generate beneficial phase transformation allows affecting the RS in a component. In
compressive RS [5–11]. While some methods affect primarily the steel fusion welding using conventional weld filler materials the
near surface material condition (e.g. peening) others may influ- ␥–␣ -phase transformation in the fusion zone (FZ) takes place at
elevated martensite start temperatures MS during cooling. Yet, the
associated material expansion is compensated by material shrink-
∗ Corresponding author. Tel.: +49 721 608 44840; fax: +49 721 608 44844. age during further cooling as schematically depicted in Fig. 1. In
E-mail address: Jens.Altenkirch@kit.edu (J. Altenkirch). conventional low and high strength structural steels this effect

0921-5093/$ – see front matter © 2011 Elsevier B.V. All rights reserved.
doi:10.1016/j.msea.2011.03.091
J. Altenkirch et al. / Materials Science and Engineering A 528 (2011) 5566–5575 5567

Table 1
Test weld designation, chemical composition in wt% and experimentally determined
transformation temperatures of the LTT alloys.

Test weld LTT alloy C Ni Cr Mn Si Fe MS (after


[14])

W8 8% Ni 0.04 8 10 0.7 0.4 Bal. 184 ◦ C


W10 10% Ni 0.04 10 10 0.7 0.4 Bal. 90 ◦ C
W12 12% Ni 0.04 12 10 0.7 0.4 Bal. 39 ◦ C

and (3) after unloading was measured and in combination with the
phase fraction of retained austenite and the macroscopic lattice
strain was determined. Supplementary lab X-ray diffraction was
used for the evaluation of the amount of retained austenite prior
to and after tensile loading by considering six diffraction lines for
the analysis, thus resulting in more reliable values for the retained
Fig. 1. Comparison of strain evolution during cooling for a conventional as well as
austenite content. Additional investigations on the microstructure
a LTT weld filler material (after [4]).
and hardness distributions before and after tensile loading were
performed in order to substantiate the strain results.
could be used theoretically in order to generate compressive RS
by applying increased cooling rates within the weld zone. How- 2. Experimental
ever, the increasing content of ␣ -phase in the heat affected zone
(HAZ) of a weld is accompanied by strong embrittlement and the 2.1. Material
increased generation of cold cracks. Therefore the limitation of
the hardness in the HAZ anticipates the generation of significant The LTT filler materials were designed according to the
compressive RS due to welding. Alternatively, the development 10%Cr–10%Ni alloy concept presented, e.g. in [17] for a high-
of special welding filler materials, the so-called low transforma- strength filler material with lowered MS -temperature. Based on this
tion temperature (LTT) materials, which exhibit a low MS , allows concept three LTT alloys with the chemical composition varying in
postponing the ␥–␣ -phase transformation to near ambient tem- terms of the Ni-content between 8% and 12% were selected. With
peratures. Consequently, the associated strain arising from this regard to the aspired application of LTT materials for welding high
transformation compensates for the thermal contraction strains strength structural steels the filler materials require an appropri-
[4,12,13] as shown in Fig. 1 and this results in reduced tensile or ate strength. This is achieved by setting the LTT-carbon content
even compressive RS in the FZ as reported by Ohta et al. [4]. The to 0.04 wt% resulting in an ultimate tensile strength of approx.
decrease in MS in such LTT filler materials is achieved mainly by 1200 MPa [18] in the pure alloy. The detailed composition and the
the alloying elements Ni and Cr. The large impact of a varying Ni- calculated theoretical [19] as well as experimentally determined
content on MS was recently shown by Kromm and Kannengiesser [14] MS -temperatures for each pure LTT-alloy are given in Table 1.
[14], who reported decreasing MS temperatures for increasing It can be seen that an increasing Ni-content results in decreasing
Ni-content. MS temperatures.
Depending on the LTT alloy and the welding parameters ten-
sile RS may be reduced or significant compressive RS generated as
shown, e.g. by Dai et al., who used neutron diffraction for the deter- 2.2. Welding
mination of the RS in 12 mm thick S960Q steel welds joined with a
conventional high-strength filler OK75.78 (MS approx. 410 ◦ C) and Stress relieved steel plates of fine grained construction steel
a LTT filler (MS approx. 280 ◦ C), respectively [15,16]. Further, it is S690Q (200 × 100 × 6 mm3 ) were preheated to 100 ◦ C and welded
reported that with enhanced formation of compressive RS in the in two layers in a 60◦ V-groove alongside the longitudinal plate edge
FZ, which results from the application of LTT weld filler materials, using manual metal arc welding. The welding current and voltage
the mechanical properties, e.g. the fatigue performance or crack were set to 87 A and 26 V, respectively, while the welding speed
initiation and propagation behaviour are improved [3,4,12]. was approx. 2 mm/s resulting in a heat input of approx. 1 kJ/mm.
However, for the successful long-term application of LTT mate- The test welds were designated according to the Ni-content of the
rials in steel welds knowledge of the stability of the RS is essential. LTT-alloy used (see Table 1).
Static and/or cyclic loading and simultaneously monitoring the The chemical composition as well as the mechanical properties
stress response is an ideal tool to simulate such in service condi- yield strength  ys , ultimate tensile strength UTS and elongation at
tions. This can be done by measuring the elastic lattice strain in situ fracture for the S690Q base metal are given in Table 2. From the
as a function of the loading condition using, e.g. neutron diffraction. welded plates dog-bone shaped tensile specimens as schematically
In this paper the behaviour of the welding induced transverse shown in Fig. 2 were produced by water jet cutting. The 90 mm long
residual lattice strain as a function of transverse (quasi) static load- tapered section was reduced from 20 to 10 mm in width. The exces-
ing in the elastic and elastic–plastic regime was investigated. Using sive over-fill at the weld surface was not removed, thus increasing
neutron diffraction the phase specific residual lattice strain as (1) the weld cross section to approx. 67 mm2 , while that of the base
induced by welding, (2) superimposed by stepwise tensile loading metal is 60 mm2 .

Table 2
Chemical composition and selected mechanical properties of S690Q base metal [18].

C Si Mn P S Cr Ni Mo Nb V B Fe

0.116 0.402 1.52 0.017 0.001 0.498 0.481 0.111 0.005 0.054 0.001 Remainder
 ys ∼ 690 MPa UTS ∼770–940 MPa Elongation at fracture 14%
5568 J. Altenkirch et al. / Materials Science and Engineering A 528 (2011) 5566–5575

Fig. 2. Schematic drawing of the tensile specimen. Fine groves perpendicular to


the tensioning direction were machined into each end in order to improve the grip
between specimen and tensile rig.

2.3. In situ neutron diffraction and tensile loading

Neutron diffraction lattice strain measurements were per-


formed at the materials science diffractometer Stress-Spec at FRM
II [20], Germany. A wavelength of  = 1.6171 Å was used and the
PSD detector positioned at 2 = 87◦ and 96◦ monitoring the {2 1 1}
␣/␣ -phase and {3 1 1} ␥-phase interference line, respectively. The
primary beam was defined by slit optics set to 1 × 4 mm2 , while a
2.3 mm radial collimator was used for definition of the diffracted
beam, thus giving a gauge volume of approx. 1 × 4 × 2.3 mm3 . The
Fig. 4. A macrograph (a) and the hardness distribution of the weld cross section of
in situ experiments were performed in transmission mode and the the test weld W10 (10 wt% Ni, 10 wt% Cr) before (b) and after (c) loading to 36 kN. The
counting time was defined using the monitor count rate detected in characteristic weld zones are indicated in each plot. The dots in plot (a) represent the
the beam path after the monochromator. This resulted in counting neutron lattice strain measurement locations while the labelled boxes (a–f) indicate
times of 150 s per point for the ␣- and ␣ -phase and 900 s for the ␥- the locations where microstructure images (Fig. 5) were taken.

phase. From the raw data a linear background was subtracted and
a Gauss function was fitted to the diffraction spectra. The resulting below the weld surface for each loading step. Due to the design of
2hkl values were converted to h k l specific lattice spacing dhkl and the tensioning rig (one grip is fixed in position, while the other one
transformed into the unit cell parameter a according to: moves) the lateral position of the weld centre line moved along
 n  the tensioning direction during loading. In order to correct for this
a = dhkl ∗ (h2 + k2 + l2 ) = ∗ (h2 + k2 + l2 ) (1) offset, the measurement data were shifted laterally by matching
2 ∗ sin hkl
the distribution curves of the FWHM of the measured interference
The electro-mechanical O-frame tensioning rig at Stress-Spec is lines. In order to determine absolute lattice strain values stress
equipped with a U3 load cell (±50 kN) from HBM and self tighten- relaxed cubes of 1.7 mm length from various positions in the weld
ing hardened grips for flat specimens [21]. The rig was mounted on cross-section were cut using a diamond wire saw (wire ø = 0.3 mm).
the instrument table, such that the loading direction, which corre- Subsequently electro polishing to approx. 1.4 mm lateral length
sponded to the weld transverse direction of the tensile specimen, was used to remove possible cutting RS. For determination of the
was aligned with the scattering vector Q as depicted in Fig. 3a. local unstrained unit cell parameter a0 the cubes were bathed in
The nominal load on each specimen was increased stepwise to the neutron beam and rotated vertically in order to achieve an
36 kN in the first cycle and in one step in the second cycle and averaging effect to reduce possible texture effects. The measure-
released as depicted in Fig. 3b. A load of 36 kN corresponds to ment positions in the tensile specimens differed slightly from those
approx. 87% of the nominal base metal yield strength (and approx. where the stress relaxed cubes were removed from. To account for
50% of the nominal pure LTT-weld filler material ultimate tensile these differences the a0 values were interpolated to positions cor-
strength). responding to the corrected measurement positions. Finally, the
The unit cell parameter a for the ␣- and ␣ -phases as well as phase specific lattice strain εli with i representing the ␣-, ␣ or
the ␥-phase for stepwise loading up to 36 kN (600 MPa) in cycle 1 ␥-phase was calculated using [22]:
and for the ␣- and ␣ -phases under direct loading up to 36 kN in
cycle 2 was determined as a function of applied load. As indicated (ai − a0i ) a0i a
εli = = = i = −1 (2)
in Fig. 4a, line scans were performed across the FZ at five depths a0i a0i a0i

Fig. 3. Image of the experimental setup for the neutron diffraction measurements of the residual and loading strains induced by welding and tensile loading, respectively
(a). The weld transverse and the loading direction are aligned with the scattering vector Q. Schematic illustration of the loading steps during the first two cycles (b).
J. Altenkirch et al. / Materials Science and Engineering A 528 (2011) 5566–5575 5569

Fig. 5. Micrographs as taken at the transition line between FZ and IHAZ (a), the transition from IHAZ to OHAZ (b) and the base metal (c) at approx. 12 mm transverse distance
from the FZ using NITAL etchant. The martensitic weld line microstructure of test weld W8 (d), W10 (e) and W12 (f) was obtained using LB1 etchant.

2.4. Retained austenite, microstructure and hardness Bloech etchant (LB1, 100 ml distilled water, 20 g (NH4 )HF2 and 0.5 g
K2 S2 O5 ).
The phase fraction of retained austenite as a function of Ni- A Shimadzu Vickers hardness tester with a test load of 100 g
content before, during and after tensioning was determined based (HV0.1 ) and an indentation time of 15 s was used for hardness test-
on the neutron diffraction data by means of correlating the inte- ing. Indents were made on the weld cross section as function of
grated intensities of the fitted {2 1 1} ␣/␣ -phase and {3 1 1} lateral distance from the weld centre line as well as from the weld
␥-phase interference lines. However, in this case texture effects surface.
may cause significant variations of the determined phase fraction
as only one orientation was measured. Therefore, supplementary 3. Results and discussion
laboratory X-ray measurements within the FZ of each weld before
and after tensile loading using Zr-filtered MoK␣ -radiation were per- 3.1. Microstructure and hardness distribution
formed for verification of the neutron diffraction measurements.
The data analysis for the laboratory X-ray measurements was Fig. 4 displays a macrograph (a) and the hardness distribution
based on the 6-line-method using the {2 0 0}-, {2 1 1}-, and {3 2 1}- (b) of the initial weld cross section of test weld W10 (10 wt% Ni,
diffraction peaks of the ␣ -phase and the {2 0 0}-, {2 2 0}-, and 10 wt% Cr) and the hardness distribution (c) after tensioning to
{3 1 1}-diffraction peaks of the ␥-phase. The spot size of the inci- 36 kN (600 MPa). The characteristic weld zones (fusion zone (FZ),
dent X-ray beam was 2 × 5 mm2 . The amount of retained austenite inner (IHAZ) and outer heat affected zone (OHAZ) and base metal)
was calculated using [23,24]: are indicated in the macrograph and their outlines superimposed
onto the hardness plots. Fig. 5 shows micrographs taken at positions
100 vol%
V =         indicated by a–f in Fig. 4a.
1+ m˛hkl I˛hkl /R˛hkl / m˛hkl / mhkl Ihkl /Rhkl / mhkl
i i i i The outlines of the weld zones correspond well with the hard-
(3) ness distribution in a way that, e.g. the slope of the transition line
between FZ and IHAZ can be clearly observed in each plot in Fig. 4.
where mhkl is the multiplicity factor, Ihkl is the integrated peak The IHAZ is adjacent to the FZ ranging from approx. 2 to 7 mm
intensity and Rhkl is the intensity factor for each individual h k l in width while the OHAZ ranges from approx. 7 to 10 mm from
interference line as defined in [23,24]. In order to minimize texture the weld centre line. In the as welded condition, the hardness in
effects the retained austenite was measured under 5 -tilt angles the IHAZ varies from approx. 250 to 300HV0.1 towards the FZ. On
(±30◦ , ±15◦ and 0◦ ) and an average value was calculated. Due to the the one (1) the high cooling rates observed close to the FZ, (2) an
increased uncertainty of the phase fraction obtained from the neu- increase in ␣ -phase fraction due to stress induced martensite for-
tron data as a result of the limited number of interference lines used mation (see Section 3.2) and (3) as a result of martensite formation
for phase fraction determination, these data were used for monitor- increased compressive lattice strain (see Section 3.4) counteracting
ing the relative change during tensile loading. On the other hand, the indentation deformation upon hardness testing (such effects
the laboratory X-ray data based on six interference lines obtained were reported before (e.g. [25]) may cause the increased hard-
prior to and after tensile loading allow for sound determination of ness values towards the FZ in this region). The OHAZ displays the
the phase fraction of retained austenite. typical softening zone indicating that the local welding tempera-
For microstructural analysis microsections of each weld before ture exceeded the tempering temperature with the consequence of
and after tensile loading were metallographically prepared. The the observed significant drop in hardness through the entire plate
macroscopic weld structure was etched using Fry etchant (100 ml thickness. The base material has a hardness of approx. 275HV0.1 .
distilled water, 120 ml HCl and 90 g CuCl2 ). Microstructure images The grain size of the post-weld martensitic-bainitic microstructure
of the base metal were obtained using light microscopy on NITAL decreases from IHAZ to OHAZ (Fig. 5a and b). The OHAZ contains
(3 ml HNO3 in 97 ml ethanol) etched weld cross sections. The horizontal bands of carbides, which coarsen due to the temperature
microstructure in the FZ was obtained using Lichtenegger und distribution during welding and were observed in each test weld.
5570 J. Altenkirch et al. / Materials Science and Engineering A 528 (2011) 5566–5575

Table 3
FZ hardness as a function of Ni-content averaged over ±2 mm from the weld centre
line at 3 mm below the weld surface before and after tensioning to 36 kN (600 MPa).
The uncertainty is the standard deviation from the measurement points over which
the average hardness was calculated.

Alloy HV0.1

As welded After tensioning

W8 (8 wt% Ni, 10 wt% Cr) 446 ± 9 439 ± 7


W10 (10 wt% Ni, 10 wt% Cr) 400 ± 8 420 ± 8
W12 (12 wt% Ni, 10 wt% Cr) 383 ± 7 396 ± 7

Such bands of carbides in fine grained steels form at normalizing Fig. 6. Intensity distribution (normalized to 1 min counting time) in the ␥-phase as
temperatures [26]. measured in the FZ for the as welded condition before loading, at maximum load of
36 kN and after unloading.
The metal in the FZ (Fig. 5d–f) contains a cellular structure with
martensitic cell cores (brownish) and presumably austenite in the
intercellular areas (light areas). The amount of retained austenite
depends on the chemical composition and rises with increasing
Ni-content [27]. Presumably, this is due to the pronounced similar
segregation of Cr and Ni during the primary austenitic solidification.
Consequently, intercellular areas with higher Cr- and Ni-content
than the cores solidify at last. The local concentration of alloy-
ing elements may suppress the ␥–␣ -phase transformation even
at ambient temperature leading to varying amounts of retained
austenite. The solidification process and the resulting microstruc-
ture are subject to further investigation.
After tensile loading to 36 kN (600 MPa) the hardness map in Fig. 7. Amount of retained austenite as function of applied loading during cycle 1 at
Fig. 4c reveals that the band of low hardness in the OHAZ dis- the weld centre line and 3 mm below the weld surface. Note, the alloy with 12 wt%
appears, while the hardness gradient from IHAZ towards the FZ Ni was loaded only to 33 kN, as necking in the HAZ occurred at this load level already
and subsequently no intermediate unloading step was performed.
reduces as it now spreads over a wider region thus decreasing the
width of low hardness zone (approx. 260HV0.1 ) in the IHAZ. The
increased hardness in the HAZ may be attributed to strain harden- martensite fraction from top to bottom is supported by the fact that
ing as the maximum tensile load exceeded the local yield strength, the hardness distribution displays the same trend (Fig. 4), namely
which was reduced as a result of the weld thermal cycle. Similar a slight increase in hardness towards the weld bottom.
observations were made in all test welds. At the maximum load of 36 kN the diffraction intensity distri-
In Table 3 the hardness of the FZ at 3 mm below the weld surface bution in the ␥-phase reveals a significant reduction at the weld
and averaged over ±2 mm from the weld centre line in each weld surface, while the root remains at a rather constant level compared
prior to and after tensioning are given. With increasing Ni-content to the initial condition. This change in intensity may be a result of
the hardness decreases, which is due to the fact that the MS tem- stress induced martensite formation, which leads to a reduction of
perature reduces and therefore the amount of retained austenite the phase fraction of retained austenite. After unloading no signifi-
increases [14,27]. As a result, a weld with an increased fraction of cant changes occur with respect to the maximum loading condition,
retained austenite has lower mean hardness. On the other hand, hence no further changes in ␥-phase fraction may arise.
the tensioning resulted in increased hardness in the FZ of test Fig. 7 compares the amount of retained austenite at the weld
welds W10 and W12 indicating stress induced martensite forma- centre line at 3 mm below the weld surface as a function of loading
tion [27]. As the phase fraction of retained austenite decreases and of the three LTT alloys tested. In the initial condition it is obvious
that of the martensitic ␣ -phase rises the hardness also increases. that with increasing Ni-content the amount of retained austenite
This observation is supported by the quantitative determination of rises. This may be attributed to the fact that the MS -temperature
the amount of retained austenite as a function of loading which is decreases as the Ni-content increases [14,27]. As a consequence
discussed in the following section. the hardness decreases as shown in Table 3.
With increased loading and up to the maximum load the phase
3.2. Retained austenite fraction of retained austenite decreases. This is most obvious in
the alloy with 12 wt% Ni which has 33% retained austenite in the
The integrated neutron diffraction intensity distribution (nor- starting condition and somewhat less in the alloy with 10 wt% Ni
malized to 1 min counting time) as measured in the ␥-phase in the (12.6% initial retained austenite). On the other hand, the alloy with
FZ for the as welded condition before loading, at maximum load of 8 wt% Ni and only 4.3% of initial retained austenite reveals a slight
36 kN and after unloading of test weld W10 (10 wt% Ni, 10 wt% Cr) increase upon loading. However, the change is within the mea-
is displayed in Fig. 6. Neutron diffraction measurements in the ␥- surement uncertainty and as such cannot be taken as a real effect.
phase were performed within the FZ only as no (retained) austenite After the maximum load, in this case 36 kN (W8 and W10) and
is present in the base metal. With respect to Fig. 6a, in the initial con- 33 kN (W12) is reached and upon unloading the phase fraction of
dition a decrease in intensity of the diffracted neutrons from weld retained austenite remains rather constant. For the investigated
surface towards the root can be observed. This may be attributed to welds this means that the less austenite is present in the FZ the
either a reduction of the phase fraction of the ␥-phase or a continu- higher is the stress necessary to cause martensite formation. This
ous change in orientation of the grains with increasing depth. While is advantageous as changes in microstructure result in variations of
the latter assumption can currently not be analysed with the lim- the mechanical properties and this should be avoided during ser-
ited neutron diffraction data (only one orientation), a reduction of vice unless such changes improve the mechanical properties as, e.g.
the phase fraction of retained austenite and therefore an increase of the yield strength, which appears to happen in the LTT alloys.
J. Altenkirch et al. / Materials Science and Engineering A 528 (2011) 5566–5575 5571

Table 4 shape of the FZ in that the width of the FZ, as marked by increased
Retained austenite before and after tensile loading to 36 kN (33 kN) as determined
a0 values, decreases with increasing depth.
using common lab-X-ray diffraction and the 6-line method (Eq. (3)). The uncertainty
is the standard deviation of the phase fractions from all possible combinations of The gradually rising uncertainty from the base metal towards
five out of the six h k l lines used for the 6-line method. the FZ is due to the fact that the grain size in the FZ increases
with respect to the base metal (Fig. 5) as well as the occurrence
Alloy Retained austenite as
determined using
of preferred grain orientation. However, the uni-axial rotation of
Mo-lab-X-ray radiation the stress relaxed cubes during diffraction measurement certainly
reduced the detrimental effects of texture to some extend. The ␥-
Before loading After loading
phase in test weld W10, which is apparent only in the FZ, does not
W8 (8 wt% Ni, 10 wt% Cr) 2.3 ± 0.6 2.0 ± 0.9 show significant variations across the weld line, however, for strain
W10 (10 wt% Ni, 10 wt% Cr) 6.3 ± 1.9 5.8 ± 1.3
W12 (12 wt% Ni, 10 wt% Cr) 37.5 ± 4.1 28.9 ± 5.8
and stress calculation knowledge of this value is fundamental. Com-
parison of the three LTT-alloys of interest reveals a slight decrease
of a0 in the weld zone in the ␣ - and ␥-phases with increasing
As given in Table 4 the same trend of reduced phase fraction of Ni-content (Fig. 8c and d).
retained austenite as a result of external tensile loading was found
using lab-X-ray diffraction applied to the as-welded sample before 3.4. Residual strain
and after tensile loading.
As only the weld transverse lattice strain was measured during
3.3. Unstrained unit cell parameter the in situ tensioning diffraction experiment, conclusions on the
residual stress may be deceptive as the strain distribution in the
The variation of the unstrained unit cell parameter a0 in the ␣- remaining directions affect the stress in the transverse orientation
and ␣ -phase (␣ in the base metal and ␣ in the weld metal) of and vice versa. Therefore, in Fig. 9a–c we show the lattice strain dis-
test weld W10 at 1, 3 and 5 mm below the weld surface is shown tribution in the ␥- and ␣/␣ -phase in the weld transverse direction
in Fig. 8a, while plot b displays the distribution in the ␥-phase in before loading, as tensioned to 36 kN (600 MPa) and after unload-
the FZ. Plots c and d compare the variation of a0 in the ␣/␣ - and ing of test weld W10 (10 wt% Ni, 10 wt% Cr) during the first cycle
␥-phase of the three LTT-alloys tested (Note: due to the very low (Note: The ␥-phase occurs only in the FZ). The strain free marten-
amount of retained austenite in the 8 wt% Ni alloy, the unstrained site in the FZ in the initial condition is characteristic for the LTT
lattice parameter in this phase was not measured as the allocated alloys investigated [18], while the IHAZ is in compression and the
beam time prohibited the necessary long counting times for statis- OHAZ in tension near the weld surface, but both reducing to zero
tically meaningful diffraction data). Due to chemical variations the lattice strain towards the weld bottom. This strain distribution pre-
value for a0 in the ␣ -phase in the weld differs significantly from sumably results from the two weld layers. While the second layer
that observed in the ␣-phase in the base metal being equivalent to is produced, the residual stresses resulting from the first layer is
approx. 1700 ␮␧ which is equivalent to approx. 370 MPa. Such high redistributed. Additionally, the width of the V-shaped FZ and as
values emphasise the importance of careful measurement of a0 for such the length over which material expansion due to martensite
strain and stress determination, especially when this value is likely formation occurs in the transverse direction reduces from the weld
to vary locally. The distribution of a0 at different depths mirrors the surface towards the weld root and as such the level of compressive

Fig. 8. The distribution of the unstrained unit cell parameter a0 in the ␣/␣ (a) and ␥-phase (b) of test weld W10 at 1, 3 and 5 mm below the weld surface and a comparison
of the a0 variation in the ␣/␣ (c) and ␥-phase (d) of the three LTT-alloys tested.
5572 J. Altenkirch et al. / Materials Science and Engineering A 528 (2011) 5566–5575

Fig. 9. The weld transverse lattice strain distribution in test weld W10 for the as welded (a), the 36 kN loaded (b) and the unloaded condition (c); respectively. The characteristic
weld zones and phases are indicated in each plot.

lattice strain in the IHAZ may also reduce towards the weld root. [28]), which indicates that the ␥-phase yield strength was exceeded
The compression is compensated by tension in the OHAZ. The ␥- and the material plastically deformed beyond an external load of
phase, which occurs only in the FZ, is completely in compression. 400 MPa. Further, when loading to the maximum of 36 kN, the
As the plates were welded without clamping, during cooling some relative variation in lattice strain in the ␣-phase changes: e.g. in
of the compressive and tensile residual lattice strain relaxed in that the IHAZ it rises by approx. 2250 ␮␧ and in the OHAZ by approx.
the plates distorted. In fact, prior to tensioning the dog bone shaped 2000 ␮␧. As a result of the high temperature cycle during weld-
test specimens displayed up to 4◦ of angular distortion. However, as ing, annealing and relaxation effects resulted in reduced local yield
displayed in Fig. 9a, a significant portion of transverse compressive strength in the HAZ as compared to the unaffected base metal.
lattice strain remains within the IHAZ. An external load of 36 kN apparently exceeds this reduced local
Naturally, upon external transverse tensile loading the lattice yield strength in the HAZ (␣-phase) and causes plastic deformation,
strain in the loading direction increases in each phase as shown while the FZ (␣ -phase) and base metal (␣-phase) are still in the
in Fig. 9b for the maximum load of 36 kN (600 MPa). The lattice elastic regime. As plastic deformation is irreversible, after unload-
strain in the ␣/␣ -phase increases by approx. 2500 ␮␧ which corre- ing the tensile lattice strain changed into compression within the
sponds to approx. 550 MPa with E˛{211} = 219.911 GPa (calculated entire HAZ and in the ␥-phase of the FZ (Fig. 9c) increased compres-
after [28]) and is nearly equal to the external load. However, in sion is observed. The amount of plastic deformation in the ␥-phase,
the ␥-phase the lattice strain rises by approx. 2250 ␮␧ only which as quantitatively determined by the change in FWHM of the h k l
is equal to approx. 400 MPa (E{311} = 177.329 GPa, calculated after interference lines as shown in Fig. 10, was greater than in the ␣/␣ -

Fig. 10. Change in transverse lattice strain (a) and FWHM (b) with respect to the as-welded condition in the ␣ - and ␥-phase in the FZ as well as the ␣-phase in the OHAZ at
7 mm from the weld centre line during cycle 1 (loading to 36 kN and subsequent unloading) in test weld W10.
J. Altenkirch et al. / Materials Science and Engineering A 528 (2011) 5566–5575 5573

Fig. 11. The weld transverse macroscopic lattice strain as calculated from the phase specific lattice strain and taken into account the local phase fraction distribution in test
weld W10 for the as welded (a) and (b) the unloaded condition respectively. The characteristic weld zones are indicated in each plot.

phase and as such the increase in compressive lattice strain is also be attributed to the local plastic elongation of the material during
greater in the ␥-phase. Fig. 10 displays the relative change of trans- tensile loading, which after unloading results in increased compres-
verse lattice strain (a) and the FWHM of the diffraction peak (b) with sion as surrounding material constrains the elongated material. The
respect to the initial condition at 3 mm below the weld surface dur- slope of the lattice strain curves during loading mirrors the Young’s
ing loading in cycle 1 in the FZ (␥- and ␣ -phase) as well as the OHAZ Modulus, which in this case is determined by a best linear fit to the
(␣-phase). The lattice strain of the ␣ -phase in the FZ returns to its strain curve given in Fig. 10a. The experimentally determined val-
starting value after unloading indicating purely elastic behaviour, ues of E˛{211} = 227.2 GPa and E{311} = 186.5 GPa are in agreement
which is in accordance to the negligible change in FWHM. On the with the literature [28] indicating that the loading experiment and
other hand, the curves for the ␣-phase in OHAZ and the ␥-phase the in situ lattice strain measurement using neutron diffraction is
in the FZ reduce in slope at approx. 24 kN (400 MPa) indicating the fairly accurate.
beginning of plastic deformation in these regions as the local yield Finally, Fig. 11 displays the distribution of the transverse macro-
strength is exceeded. This is supported by the fact that the FWHM scopic lattice strain for the condition before loading (a) and after
starts to increase at these load levels and continuously rises until unloading from maximum load of 36 kN of test weld W10 (10 wt%
maximum loading is reached, which indicates a continuous gain Ni, 10 wt% Cr). The macroscopic lattice strain was calculated based
in dislocation density as a result of ongoing plastic deformation. on a simple mixture rule:
Further, at the point when yielding of the ␥-phase starts and the 
slope of the corresponding stress–strain curve reduces, that of the εl
i i
∗ Vi
ε= (4)
␣ -phase curve in the FZ increases indicating that the martensitic 100
phase is stressed with a higher portion of the external load. which correlates the phase specific lattice strain εli with the phase
After unloading the lattice strain curve reveals increased com- specific volume fraction Vi as calculated using Eq. (3). The macro-
pression in the ␥-phase in the FZ and ␣-phase in the OHAZ. This may scopic lattice strain distribution in the base metal, the OHAZ and

Fig. 12. The change in macroscopic lattice strain 3 mm below the weld surface after loading to maximum load of 36 kN (33 kN in case of W12). Due to beam time limitations
neutron measurements were performed only up to 8 mm from the weld centre line in test weld W12.
5574 J. Altenkirch et al. / Materials Science and Engineering A 528 (2011) 5566–5575

IHAZ is identical to that shown in Fig. 9 as only the ferritic ␣-phase increasing number of loading cycles material fatigue may result in
material is present and the change in lattice strain in these regions further changes. This remains to be investigated in future work.
as a result of external loading was discussed before. However, the
macroscopic lattice strain distribution in the FZ is affected by the ␣ -
4. Conclusions
and ␥-phase lattice strain as a function of the phase fraction of each
phase. In the condition before loading the macroscopic lattice strain
In this paper the response of the weld transverse residual lat-
in the FZ is approx. 130 ␮␧ less than in the martensitic ␣ -phase,
tice strain to external tensile loading of welds joint with LTT weld
which results from the 12.6% retained austenite which has approx.
filler materials with varying Ni-content (8–12 wt%) was investi-
−1000 ␮␧. After loading the phase fraction of the ␥-phase reduces
gated. In addition to the in situ lattice strain measurements using
to approx. 5% due to stress induced martensite formation while the
neutron diffraction, the hardness and microstructure distributions
compression in the ␥-phase increases to approx. −2000 ␮␧. There-
were characterised and the amount of retained austenite prior to
fore, the input to the macroscopic lattice strain resulting from the
and after tensile loading was determined. From these experimental
␥-phase is nearly the same, namely approx. −100 ␮␧ and as such
investigations the following conclusions may be drawn:
the change in macroscopic lattice strain as a result of external load-
ing depends mainly on the martensitic ␣ -phase. As this phase was
elastically loaded only, no significant change in macroscopic lat- • The residual lattice strain distribution of the base metal was
tice strain occurs. In case of test weld W10 the compressive region not affected by the external tensile loading, as the maximum
between FZ and IHAZ increased in lateral width as well as in magni- load of 600 MPa was well below the base metal yield strength
tude though narrowing the strain plateau in the FZ, which remains  YS = 690 MPa.
in slight compression. In the OHAZ, which has the lowest hardness • Within the IHAZ and OHAZ the lattice strain distribution changed
(Fig. 4) and hence yield strength, is substantially affected by tensile significantly. Due to the weld thermal cycle this region was soft-
loading and the lattice strain shifts from tension into compression. ened and the applied stress exceeded, the local lowered yield
The base metal remains almost unaffected. strength resulting in plastic elongation. After unloading the lat-
A direct comparison of the change in macroscopic lattice strain tice strain was shifted to higher compression compared to the
at 3 mm below the weld surface determined from the condition initial condition.
before and after loading to maximum load for the three LTT alloys • The assumption of plastic deformation within the HAZ is sup-
investigated is shown in Fig. 12. As discussed before, the transition ported by increasing hardness and increasing values of the FWHM
zone between IHAZ and OHAZ ranging from 6 mm to 8 mm from the of the interference lines, which are both indicators for an increase
weld centre line undergoes a substantial shift towards compression in dislocation density due to plastic deformation. Further, necking
as a result of plastic deformation within this region as the local yield as observed on the surface of the tensioning specimen strength-
strength is exceeded by the external stress. The base metal remains ens the assumption that plastic deformation occurred in this
more or less unaffected because the maximum load of 36 kN (33 kN region.
in case of W12), which is equal to 600 MPa (550 MPa) within the • With increasing Ni-content the amount of retained austenite in
base metal cross section, is approx. 87% (approx. 80%) of the base the FZ increases, which is due to the fact that the MS -temperature
metal yield strength and as such purely elastic behaviour occurred. decreases with increasing Ni-content [14,27] and as a result the
In opposite to the comparable lattice strain behaviour occurring hardness decreases.
in the IHAZ, the OHAZ and the base metal in all three test welds, • Further, with increasing depth in the FZ the amount of retained
the changes in macroscopic lattice strain within the FZ vary for austenite reduces, while the hardness increases. This may be
each alloy tested. In test weld W8 (8 wt% Ni, 10 wt% Cr) a shift by attributed to annealing effects within the weld root during weld-
approx. 180 ␮␧ from tension into compression occurred after load- ing of the second layer causing retained austenite to dissolve.
ing. As the amount of retained austenite is negligible, this may be Also, chemical dilution near the transition zone (LTT to base
attributed to plastic deformation of the martensitic FZ material. metal) results in higher transformation temperatures and as such
As shown in Fig. 9 the external loading of test weld W10 (10 wt% less retained austenite remains.
Ni, 10 wt% Cr) resulted in substantially increased compression in • As a result of external transverse tensile loading stress induced
the ␥-phase while at the same time the phase fraction of retained martensite transformation occurs resulting in decreasing phase
austenite reduced. The lattice strain in the martensitic ␣ -phase fraction of retained austenite in the FZ. This effect was greatest
remained constant, but the width of the FZ lattice strain plateau in the test weld W12 with 12 wt% Ni and 10 wt% Cr, which has
reduced slightly. Overall the reduced impact of the increased com- the highest initial fraction of retained austenite. Along with the
pressive lattice strain of the ␥-phase due to the reduction in phase reduction of retained austenite the hardness in the FZ increased.
fraction resulted in a negligible reduction in macroscopic lattice This is a significant advantage as the in-service component per-
strain in the FZ in W10. formance may improve as a result of the applied load.
Finally, in test weld W12 (12 wt% Ni, 10 wt% Cr) the FZ reveals a • The retained austenite in the FZ starts to elongate plastically
significant shift towards compression as a result of external load- at tensioning levels well below the maximum load. As a result,
ing. This may be attributed to the fact that the ␥-phase material within the elastically strained martensitic matrix, the plastic
is plastically stressed and within the martensitic structure this elongation of the ␥-phase results in increased compressive lattice
results in increased compression. Even though a significant por- strain after unloading.
tion transforms into martensite as a result of the applied stress, the • The transverse macroscopic lattice strain in the FZ revealed a
influence of the increased compression on the macroscopic lattice nearly strain free condition after welding. Due to tensile load-
strain remains. In addition, the significant formation of martensite ing the ␥-phase fraction reduces due to strain and stress induced
results in increased compression within the FZ. martensite formation. At the same time the compressive lattice
With respect to the second loading cycle with just one step to strain increases. These two effects appear to balance out in case
maximum load only (Fig. 3), no differences in the lattice strain dis- of test weld W10 (10 wt% Ni, 10 wt% Cr), where no significant
tribution were observed during and after loading and therefore the change in macroscopic lattice strain was observed after tensile
results are left out at this point. However, this invariant means that loading. On the other hand in the weld with higher initial amount
unless the applied load increases beyond that of the first cycle the of retained austenite (W12) a clear increase in compressive lattice
mechanical properties remain constant. On the other hand, with strain was observed.
J. Altenkirch et al. / Materials Science and Engineering A 528 (2011) 5566–5575 5575

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