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Fusion Engineering and Design 82 (2007) 26152620

Investigation of the susceptibility of EUROFER97 in


leadlithium to liquid metal embrittlement (LME)
R.W. Bosch , S. van Dyck, A. Al Mazouzi
SCK-CEN, Belgian Nuclear Research Centre, Boeretang 200, B-2400 Mol, Belgium
Received 7 August 2006; received in revised form 2 April 2007; accepted 2 April 2007
Available online 29 May 2007

Abstract
Liquid metal embrittlement (LME) is defined as the brittle fracture (loss of ductility) of usually ductile materials in the presence
of a liquid metal. The sensitivity to LME is likely to increase with irradiation hardening as localised stresses can promote the
aggressive action of a liquid metal. To investigate the mechanical response of irradiated materials in contact with a liquid metal,
an instrumented hot cell has been developed. The testing machine installed inside allows mechanical testing of active materials
in liquid lead lithium under well controlled chemistry conditions. Typical mechanical tests that can be carried out are slow strain
rate tests (SSRT), constant load and rising load tests at temperatures from 150 C to 500 C. In this paper the first results of the
SSRT tests with EUROFER97 in argon and leadlithium at different temperatures with different strain rates will be presented.
The SSRT test method has been chosen due to the accelerated nature of the test, i.e., during straining the oxide layer will be
ruptured and wetting of the sample surface by the leadlithium melt is promoted. The results collected up till now showed no
sign of LME. Tests with longer pre-exposure times and tests with irradiated samples will be carried out in the next phase. A
longer pre-exposure time can enhance wetting and so the susceptibility to LME. An increase of the yield stress due to irradiation
can also enhance the susceptibility to LME.
2007 Elsevier B.V. All rights reserved.
Keywords: LME; SSRT; Hot cell; Leadlithium

1. Introduction
Reduced activation steels have been developed for
application in new reactor concepts, where high neutron fluxes and long life times are anticipated. Within
the framework of the European Fusion Development

Corresponding author. Tel.: +32 14 333428.


E-mail address: rbosch@sckcen.be (R.W. Bosch).

0920-3796/$ see front matter 2007 Elsevier B.V. All rights reserved.
doi:10.1016/j.fusengdes.2007.04.006

Association, a 9%Cr1%W steel has been defined,


the EUROFER97 steel. In the current design concepts there are two potentially corrosive environments
for this type of material, namely water at high temperature and liquid leadlithium eutectic alloy. The
corrosion behaviour (susceptibility to stress corrosion
cracking) of EUROFER97 in high temperature water
has been studied for unirradiated [1] and irradiated
materials [2]. In leadlithium another failure mecha-

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nism is possible, so-called liquid metal embrittlement


(LME).
Liquid metal embrittlement (LME) is defined as
the brittle fracture (loss of ductility) of usually ductile
materials in the presence of liquid metal. The sensitivity to LME is likely to increases with irradiation
hardening [3,4]. Therefore, a hot cell slow strain rate
test set-up has been developed (so-called LIMETS2),
which allows testing of active materials in liquid metal
like leadlithium and lead-bismuth. The test set-up will
be designed in such way that tests can be performed in
both leadlithium (related to the fusion research) as
in lead-bismuth (related to the MYRRHA program)
[5,6]. As leadlithium is a reducing system and so easier to be removed from the interior of the test set-up,
tests will first be carried out in leadlithium and then
in lead-bismuth. The conditioning systems are slightly
different, but will both be integrated in the design.
The main characterization of LME is the very high
crack growth rate, being in the range of 1 cm to several
meters per second [6]. Therefore, the main emphasize
of LME investigation has been on initiation assuming
that when LME starts, the construction has reached end
of life. Due to these very high crack growth rates, little
or no attention has been given to fracture mechanics
type of testing. In case of smaller crack growth rates a
fracture mechanics approach would certainly increase
our understanding of the phenomena [7,9,10]. It has
also been stated that local stress concentrations or stress
raisers might be a requirement for LME to start/run
[68]. So when defining the type of mechanical testing
to be carried out, we did not only look at initiation tests
but also at fracture mechanics testing. The following
tests are considered to be important.

Slow strain rate tests (SSRT) [11].


Constant load.
Rising load.
Crack growth rate (fracture mechanics).

Previous work showed that unirradiated EUROFER97 is not very sensitive to LME in leadlithium
eutectic. Only a few studies have been carried on LME
in Pb17Li. Cone showed that no LME was found for
stainless steel 316L at temperatures close to the melting
point of leadlithium [12]. Tests with notched tensile
specimens at 350 C under a constant uniaxial tensile
load, below the engineering yield stress, however have
evidenced that many cracks filled with Pb and possibly

Li were formed, not excluding a liquid metal embrittlement effect [13]. Borgstedt showed that with low cycle
fatigue tests with a martensitic steel there was no occurrence of LME [14] A reduced life time for this steel
during creep tests could only be observed for long exposure times, but was related to the reduced diameter of
the specimens. Martensitic steels were tested in P17Li
at 250 C by Sample and it was shown that there was no
LME in the tempered condition [15]. Tests of the heat
affected zone shows a LME susceptibility at 250 C,
while increasing the test temperature up to 400 C led
to a recovery of the ductility. Post-weld treatment was
sufficient to recover the mechanical properties. Concluding, LME could be found when materials are in the
hardened condition (HAZ) and when there is a stress
concentrator (notch). In this work the EUROFER97
samples are in the as-received conditions.
In this paper the first results of the SSRT tests with
EUROFER97 in argon and leadlithium will be presented. This SSRT technique is used to investigate the
susceptibility of a metal or alloy to stress corrosion
cracking in a certain corrosive environment. According to the ASTM-standard G 129-95 [11] the results
of a SSRT experiment are not intended to necessarily represent service conditions, due to the accelerated
nature of the test. However, it provides a basis for
screening, for detection of an environmental interaction with a material, and for comparative evaluation of
the effects of metallurgical and environmental variables
on sensitivity to known environmental cracking problems. The SSRT test method has been chosen due to
the accelerated nature of the test, i.e., during straining
the oxide layer will be ruptured and wetting of the sample surface by the leadlithium melt is promoted. The
susceptibility to LME is then expressed as a difference
in mechanical behaviour in argon and leadlithium.

2. Experiment
The LME test set-up consisted of three vessels;
besides the autoclave and loading unit two more vessels
are used to prepare a test (see Fig. 1). The first vessel
(melting tank) is only used to melt the lead mixture for
the first time. Impurities and the always present oxide
layer on top of the liquid metal can be removed. This
vessel remains outside the hot cell. The second vessel
(dump tank) is used to condition the liquid metal with

R.W. Bosch et al. / Fusion Engineering and Design 82 (2007) 26152620

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Fig. 1. Simplified flow sheet of the LME slow strain rate test set-up; (1) melting tank, (2) dump tank and (3) autoclave.

a gas, for example argon or hydrogen. After the conditioning, the liquid metal mixture is ready to be used for
testing. Part of this set-up consists of a vacuum pump
and an argon gas supply, which are used to prevent the
contact of liquid metal with air and humidity. Tensile
tests can be performed with a loading unit allowing
strain rates in the range of 103 107 s1 with a maximum load of 20 kN. Fig. 2 shows the part of the set-up
that stays in the hot cell. Table 1 shows the technical
specifications.
A typical test is then performed as follows. The first
vessel (melting tank) is filled with solid particles of
lead. Then the melting tank is heated to melt the lead.
Melting can be performed under argon atmosphere.
Then the melted lead is transported to the second vessel
(dump tank) leaving the oxides formed during melting in the first vessel. A small over pressure is used
to move the liquid metal from the melting tank (1)
to the dump tank (2). From the dump tank, the lead
melt can be transported to the autoclave (3) in the same
way. A tensile specimen will be positioned in the tensile rig. This rig is present in the autoclave (3). Then
the autoclave is filled with the melted lead and a slow
strain rate tensile test can be carried out. Notice that the
liquid leadlithium is static, i.e., there is no forced
convection in the autoclave. When this tensile test is fin-

ished, the lead melt is brought back to the dump tank.


A new test campaign can be started using the lead melt
in the dump tank. Pre-exposure time of the samples
was always 30 min. The total test time then depends on
the strain rate used. For a strain to failure of 20% (see
stressstrain curves in Figs. 3 and 4) and a strain rate
104 s1 this is approximately 30 min, for a strain rate
105 s1 this is approximately 30 min and for a strain
Table 1
Specifications LME SSRT test set-up (LIMETS2)
Temperature
Pressure
Maximum load
Displacement rates
Strain rates (gage length
10 mm)
Maximum displacement
Specimens to be tested
Number of autoclaves and
loading units
Autoclave volume
Dump tank volume
Melting tank volume
Construction materials
Conditioning gasses

Max. 550 C
Max. 4 bar
20 kN
9 102 to
3 106 mm s1
9 103 to 3 107 s1
30 mm
Tensile specimen,
compact tension, O-ring
1
3.6 l
5.3 l
9.6 l
316 L
Hydrogen, argon

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Fig. 2. Schematic of the LIMETS2 with autoclave, dumptank, tensile machine and gas control panel.

rate 106 s1 this is approximately 3000 min. A test


with a pre-exposure test of 40 days is in preparation.
The leadlithium eutectic mixture was made in
house. Liquid lithium was added to liquid lead at a
temperature of 400 C under argon atmosphere. Then
this was mixed sufficiently and heated up to 600 C
(PbLi has a melting pint of 482 C) were it stayed for
at least 2 h. The mixture was could down and the eutectic temperature (235 C) could be verified. Chemical
analysis showed that the Li concentration was between
0.6 and 0.8 wt%, i.e., 0.7 wt% Li is equal to 17 atom%

Table 2
Test matrix EUROFER97, unirradiated smooth tensile specimen
Concentration (g/g)
Pb
Li
Cr
Ni
Fe

Bal.
60008000
<1
1.4
<100

R.W. Bosch et al. / Fusion Engineering and Design 82 (2007) 26152620

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Fig. 3. Influence of the temperature on LME of EUROFER97, strain rate 104 s1 .

Fig. 4. Influence of the strain rate on LME of EUROFER97, T = 250 C.

Table 3
Test matrix EUROFER97, unirradiated smooth tensile specimen
T ( C)

250
300
400

Strain rate (s1 )


Inert gas

Pb-17Li

Inert gas

Pb-17Li

Inert gas

Pb-17Li

10E4
10E4
10E4

10E4
10E4
10E4

10E5

10E5

10E6

10E6

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Li. Table 2 shows the initial composition of the Pb17Li


used.

of the yield stress due to irradiation can also enhance


the susceptibility to LME.

3. Results and discussion

Acknowledgement

SSRT tests were carried out at different temperatures


and strain rates. In this way the most critical test condition could be found, which will later on be used for the
irradiated samples. Table 3 shows the test matrix for
the unirradiated samples. Irradiated samples with irradiation dose ranging from 0.06 to 2.29 will be tested
in the next phase. The highest susceptibility to LME is
generally found just above the melting temperature of
the liquid metal. Therefore, 250 C has been chosen as
the lowest test temperature. The strain should be low
enough to allow LME to take place but high enough
to avoid crack tip blunting due to dissolution of metals
atoms. The results of the test matrix have been summarized in Figs. 3 and 4. In Fig. 3 the influence of the
temperature is highlighted. It is clear from this graph
that there is no evidence of LME under the given test
conditions. Only the influence of the temperature on the
ultimate tensile strength can be noticed. In Fig. 4 the
influence of the strain rate is highlighted. Again there
is no clear evidence of LME under these test conditions. It must be emphasized that a longer pre-exposure
time, which enhances the optimal wetting of a sample,
might change the picture. At this stage we do not think
that wetting has occurred as there is no evidence for
LME. A pre-exposure test is in preparation to tackle
this aspect. Also an increase of the yield stress due to
irradiation hardening might enhance the susceptibility
to LME. This will become clear when the irradiated
samples have been tested.

This work, supported by the European Communities under the contract of Association between
EURATOM/TTMS-003 in association with the Belgian State, was carried out within the framework of
the European Fusion Development Agreement. The
views and opinions expressed herein do not necessarily
reflect those of the European Commission. The authors
wish to thank Mr. L. Eysermans for the technical assistance during the tests with and the development of the
LIMETS2 test set-up.

4. Summary and conclusions


SSRT tests with EUROFER97 have been carried out
in Pb17Li with different strain rates at different temperatures. The results collected up till now showed no
sign of LME. Tests with longer pre-exposure times and
tests with irradiated samples will be carried out in the
next phase. A longer pre-exposure time can enhance
wetting and so the susceptibility to LME. An increase

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