Journal of Nuclear Materials 442 (2013) S204–S207

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Journal of Nuclear Materials

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Charpy impact properties of pure tungsten plate material in as-received

and recrystallized condition (1 h at 2000 °C (2273 K))
J. Reiser a,⇑, M. Rieth a, B. Dafferner a, A. Hoffmann b
a
Karlsruhe Institute of Technology, IAM-AWP, P.O. Box 3640, 76021 Karlsruhe, Germany
b
PLANSEE SE, Reutte, Austria

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

Article history: The aim of this paper is to assess the fracture behavior of tungsten plate material. Plate material with a
Available online 8 November 2012 thickness of 1 mm and 4 mm was investigated, considering samples with dimensions of 1  3  27 mm3
without notch, 3  3  27 mm3 without notch, and 3  4  27 mm3 with a 1 mm notch (KLST). The plate
material was in either as-received or recrystallized condition (annealed for 1 h at 2000 °C (2273 K)). All
samples were characterized by means of Charpy impact tests, which were performed up to 1000 °C
(1273 K) in a vacuum. The results show that plate material is anisotropic and that the brittle-to-ductile
transition temperature (BDTT) strongly depends on the orientation of the specimen. A comparison of the
results of notched and unnotched samples shows that delamination behavior only appears on notched
samples and that unnotched samples show the classical brittle-to-ductile transition (BDT). Furthermore,
it is shown that recrystallized tungsten plate material is extremely brittle and that the BDT does not even
appear at a test temperature of 1000 °C (1273 K).
Ó 2012 Elsevier B.V. All rights reserved.

1. Introduction
Tungsten and tungsten alloys are currently considered as candi-
date materials for various divertor applications in future fusion
reactors [1–3]. This is mainly due to their high temperature
strength, good thermal conductivity, and comparatively low
activation under neutron irradiation. On the other hand, the disad-
vantage of tungsten is its low fracture toughness and a brittle-
to-ductile transition (BDT) that, unfortunately, occurs at high
temperatures. This is why tungsten is used only as a functional
material but not as a structural material, which means it is not
used for safety-relevant, pressurized parts. Consequently, when
considering tungsten as a structural material, one has to address
the question of how to make tungsten ductile.
Among the commercially available tungsten materials, such as
W-1 wt.% La2O3 (WL10, see PLANSEE SE) or W-0.005 wt.% K
(WVM, see PLANSEE SE), it can be concluded that pure tungsten
is the most ductile tungsten [4–6] (measured by Charpy impact
test, with the exception of tungsten–rhenium) and that pure tung-
sten is the best choice of material for benchmark experiments. This
is why the results obtained in this work are the benchmark exper-
iments for our new tungsten material – a tungsten laminate. It was
shown in our previous work that we succeeded in extending the
ductile properties of a tungsten foil to the bulk by synthesizing a
⇑ Corresponding author.
E-mail address: jens.reiser@kit.edu (J. Reiser).
tungsten laminate [7,8]. There have been other attempts to ductil-
ize tungsten, for example by the synthesis of a tungsten solid solu-
tion [9], an ultra fine grained microstructure [10], or a tungsten
composite reinforced by particles [11] or short [12] or long fibers
[13,14]. However, the success of these attempts was limited or
the work is still in progress.
The fracture behavior of pure tungsten has been very well stud-
ied for single crystals [15–17], pre-deformed single crystals [17],
and polycrystalline rod material [4,18–20]. The aim of this work
is to investigate polycrystalline plate material in order to show
the influence of (i) the thickness, (ii) the sample orientation (L–S,
T–S, L–T, or T–L), and (iii) the notch on the impact bending
properties. Finally (iv) the behavior of recrystallized tungsten plate
material will be investigated.
2. Experimental procedure
2.1. Materials and microstructure
The material chosen for experimental investigation is rolled
unalloyed 99.97% pure tungsten plate material. The plate material
has a thickness of either 1 mm or 4 mm. This commercially avail-
able material was produced by PLANSEE Metall GmbH, Reutte,
Austria. After sintering, the plate was hot- and cold-rolled with a
high degree of deformation resulting in flat and elongated grains.
The optical micrograph of a longitudinal section of rolled tungsten

0022-3115/$ - see front matter Ó 2012 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.jnucmat.2012.10.037
 J. Reiser et al. / Journal of Nuclear Materials 442 (2013) S204–S207
Fig. 1. Nomenclature of the sample orientation: ‘‘L’’ stands for longitudinal, ‘‘T’’ for
transverse, and ‘‘S’’ for short transverse. The first letter indicates the direction
perpendicular to the expected crack plane while the second stands for the direction
of the expected crack growth.
plate can be seen elsewhere [5,6]. The rolling direction of the plate
was specified by the producer.
The recrystallized tungsten plate material that was assessed in
this work has a thickness of 4 mm and was annealed for 1 h at
2000 °C (2273 K) in hydrogen. The resulting microstructure shows
grains of the dimensions 30  30  30 lm3 (see Fig. 7).
The nomenclature of the sample orientation is as follows (see
Fig. 1): ‘‘L’’ stands for longitudinal, which means in the rolling
direction (defined as 0°), ‘‘T’’ stands for transverse, which means
perpendicular to the rolling direction (defined as 90°), and ‘‘S’’
stands for short transverse, which is the direction of the thickness
of the plate. The first letter indicates the direction perpendicular to
the expected crack plane while the second letter stands for the ex-
pected direction of crack growth.
As-received samples made from 1 mm plate material had
dimensions of 1  3  27 mm3, were without notches, and were
orientated in L–S and L–T directions. As-received samples made
from 4 mm plate material had dimensions of 3  3  27 mm3 and
were without notches and orientated in L–S, T–S, L–T, and T–L
directions or had dimensions of 3  4  27 mm3, a 1 mm notch
(KLST), and orientation in L–S and L–T directions. Recrystallized
samples made from 4 mm plate material had dimensions of
3  3  27 mm3 and were without notches and orientated in L–S
direction or dimensions of 3  4  27 mm3, a 1 mm notch (KLST),
and orientation in L–S direction. All samples were cut by electrical
discharge machining (EDM).
2.2. Charpy impact tests
Charpy tests were performed based on the EU standards DIN EN
ISO 148-1 and 14556:2006-10. According to these standards, small
size specimens have the following dimensions: 3  4  27 mm3,
22 mm span, 1 mm notch depth, and 0.1 mm notch root radius
(KLST). The striker hit the side which the EDM cut first. To avoid
oxidation, the whole Charpy testing machine (a drop-weight de-
sign) was placed inside a vacuum vessel which operates at typical
pressures of about 103 mbar. The specimen is heated together
with the support, which allows easy and precise test temperature
control. To prevent the delicate strain-gauges in the instrumented
striker from overheating, the drop-weight is catapulted out of the
furnace immediately after the test by a spring device and is then
arrested [5]. For each test temperature one sample was tested.
3. Results and discussion
Fig. 2 shows the results of the impact bending tests of
unnotched specimens with dimensions of 1  3  27 mm3 and
3  3  27 mm3 respectively.
Analyzing the results of unnotched specimens we can see a clas-
sical BDT which is characterized by brittle fracture at low temper-
atures and a clear transition to ductile material behavior at higher
S205
Fig. 2. Results of unnotched specimens. Unnotched samples show the classical
BDT: brittle at low temperatures and a clear transition to ductile material behavior
at higher temperatures. Delamination does not occur.
temperatures. The samples do not delaminate. This is astonishing,
as it was shown on KLST specimens made from rod material in L–R
orientation that tungsten does not show a classical BDT. Moreover
tungsten has two transitions: the brittle-to-delamination and the
delamination-to-ductile transition [6].
Furthermore the results in Fig. 2 shows that the BDT is a func-
tion of the sample orientation. For a 1 mm specimen orientated
in rolling direction (L–S) the BDT occurs at 200 °C (473 K); for a
1 mm specimen orientated perpendicular to the rolling direction
(T–S) the BDT occurs at 350 °C (623 K). This result can certainly
be attributed to the microstructure of the tungsten plate.
By changing the strain rate it is possible to determine the acti-
vation energy for both orientations according to
e_ p ¼ a expðDHBDT =kT BDT Þ ð1Þ
where A is a constant, k is the Boltzmann constant, and DHBDT is the
activation energy for the BDT [15]. In an Arrhenius plot of the strain
rate versus 1/TBDT, we have now determined two points: one for the
L–S direction and one for the T–S direction. This result indicates
that, by continuing the experiments on tungsten plate material with
different strain rates, in an Arrhenius plot of the strain rate versus 1/
TBDT there would be two lines which are not congruent as was re-
ported for other tungsten materials elsewhere [15,16]. One can ex-
pect these two lines to be parallel and to have the same slope,
which means that the BDT activation energy is equal in both cases.
Comparing the results of 1 mm and 3 mm specimens, one can
see that the upper shelf energy (USE) differs by a factor of 10.
The USE of a 1 mm specimen is about 1 J and that of a 3 mm spec-
imen about 10 J. This result can easily be attributed to the section
modulus W (m3), according to
bh3 2
1 12 bh
W¼ ¼ ¼ ð2Þ
amax 2
h 6
where I (m4) is the moment of inertia, amax (m) is the maximum dis-
tance from the neutral axis, b (m) is the width and h (m) is the
height of the sample. So it can be maintained that:
W 1327 USE1327
3327
 ð3Þ
W USE1327
Furthermore the comparison of the results of 1 mm and 3 mm
specimens shows a shift of the BDT to lower temperatures.
One reason for this behavior is the strain rate. The strain rate
S206 J. Reiser et al. / Journal of Nuclear Materials 442 (2013) S204–S207
Fig. 3. Results of unnotched specimens. The BDT for samples orientated in L–S and
L–T directions as well as for samples orientated in T–S and T–L directions occurs at
the same temperature.
Fig. 4. Fractured surfaces of unnotched specimens. Even if the BDT occurs at the
same temperature the fractured surfaces look different. In the fractured surfaces of
L–T and T–L samples the elongated grains are visible (see arrows).
Fig. 5. Results of Charpy test of notched samples (KLST). Samples orientated in L–S
direction show delamination fracture; samples orientated in L–T direction show
facetted fracture surfaces.
dependence of tungsten is well known [15,17]. Due to the geome-
try the strain rate of the 1 mm specimen is smaller than that for a
3 mm specimen by a factor of three. However a shift of 200 K in the
BDTT cannot be explained by an increase in the strain rate by a fac-
tor of three. It is highly probable that this result is mainly due to
the microstructural change. The 1 mm tungsten plate was exposed
to a higher degree of cold work, resulting in a microstructure of
smaller grains as well as a higher amount of mobile edge disloca-
tions. Both small grains and a large amount of mobile edge disloca-
tions might be responsible for the shift of the BDT.
Fig. 2 also shows the results for recrystallized specimens. The
sample cannot dissipate energy even at a test temperature of
1000 °C (1273 K). The sample failed by intergranular fracture. This
result show that for safety-relevant parts made of tungsten plate
material recrystallization has to be avoided under any
circumstances.
Fig. 3 shows the results of Charpy impact tests of samples with
dimensions of 3  3  27 mm3 without notches. The samples were
orientated in L–S, T–S, L–T, and T–L directions. Again all samples
show the classical BDT and no delamination. Furthermore all sam-
ples orientated in the rolling direction (L–S and L–T) have the same
BDTT, which is at 400 °C (673 K). This is astonishing as the striker
of the test device hits the grains on the flat side in one case (L–S)
and on the narrow side in the other (L–T). Furthermore the frac-
tured surfaces of the L–S and L–T samples look different too (see
Fig. 4).
Similar results can be obtained for samples orientated perpen-
dicular to the rolling direction (T–S and T–L). For both orientations
the BDTT is at 500 °C (773 K) and the fractured surface can be seen
in Fig. 4.
The results of notched samples (3  4  27 mm3, 1 mm notch,
KLST) can be found in Fig. 5. Now the samples tested in L–S orien-
tation show delamination fracture as was reported for L–R samples
made from rod material [6]. Fig. 6 shows the tested samples and
gives an impression of what delamination fracture looks like. It
can be concluded that the transition from brittle to delamination
occurs at 500 °C (773 K), whereas the transition from delamination
to ductile does not even appear at a test temperature of 1000 °C
(1273 K). Comparing the results of unnotched samples orientated
in L–S direction from Fig. 1, it can be concluded that delamination
only occurs for notched samples. This difference in the fracture
behavior cannot be attributed to the microstructure as both sam-
ples were made from 4 mm plate material. Rather the combination
of the microstructure and the three-dimensional stress state of
notched samples must be responsible for the different fracture
behavior.
During a Charpy test a three-dimensional stress state is estab-
lished at the notch base. The maximum stress occurs in the longi-
tudinal direction of the sample (y-direction). But there is also stress
in the direction of the thickness of the sample (x-direction) which
has its maximum not in the notch base but at a small distance from
the notch [21]. It was shown by samples in the L–R orientation
made from tungsten rod material that the crack starts not in the
notch base but in the sample [19], exactly where the maximum
x-stress appears. The crack now penetrates nearly parallel to the
sample surface; that is, delamination occurs [19,20]. In the case
of an unnotched sample there is quite a simple stress state. But
as soon as a crack appears, a three-dimensional stress state is
established too. This three-dimensional stress state was responsi-
ble for the delamination behavior. This is why delamination should
also appear in unnotched samples. But it does not. So unnotched
samples do not show a semi-brittle regime.
The comparison of the results of notched samples (KLST) in L–S
and L–T orientations gives further proof of the anisotropic material
behavior of tungsten and the strong influence of the microstruc-
ture on the fracture behavior of tungsten. While the samples
 J. Reiser et al. / Journal of Nuclear Materials 442 (2013) S204–S207
Fig. 6. Notched samples, orientated in L–S direction, have two transitions: one from brittle to delamination and one from delamination to ductile. Unfortunately the
transition from delamination to ductile does not even appear at 1000 °C (1273 K).
Fig. 7. Fractured surface of a Charpy test sample made from recrystallized tungsten
plate material. The fracture is intergranular and the grains have dimensions of ca.
30  30  30 lm3.
orientated in L–S direction show delamination fracture the sam-
ples orientated in L–T direction show a facetted fracture surface
(see [4–6]). This facetted fracture surface can also be found in
rolled oxide dispersion strengthened (ODS) reduced activation fer-
ritic (RAF) steels [22]. This is why it can be predicted that the frac-
ture behavior of tungsten, characterized by delamination of L–S
samples and facetted fracture surfaces of L–T samples, also occurs
in ODS RAF steel.
Finally, Fig. 5 shows the result of a recrystallized test sample, L–
S. Even at a test temperature of 1000 °C (1273 K) this sample could
not dissipate energy. The fracture surface shows an intergranular
fracture and gives an impression of the grain size.
4. Summary
Among all commercially available tungsten materials, pure
tungsten is the most ductile (measured by Charpy impact test, with
the exception of tungsten-rhenium). This is why the results of the
characterization of pure tungsten material can be regarded as
benchmark experiments for new ductile tungsten materials such
as tungsten laminate.
In this paper the fracture behavior of tungsten plate material
has been investigated by means of Charpy impact tests. It was
shown on unnotched specimens that the BDTT depends on
whether the sample is orientated in the rolling direction or perpen-
dicular to the rolling direction. This shows that in an Arrhenius plot
of the strain rate versus 1/TBDT there would be two lines which are
not congruent.
The comparison of the results of unnotched 1 mm and 3 mm
specimens shows a shift of the BDTT of 200 K. This result cannot
be explained solely by an increase in the strain rate by a factor of
S207
three. It is highly probable that this result is mainly due to the
microstructural changes that are established during cold work,
for example the appearance of smaller grains and a higher amount
of mobile edge dislocations.
Furthermore it was shown that delamination fracture only ap-
pears on notched samples and that the delamination fracture can-
not be attributed to the microstructure alone but is also due to the
combination of microstructure and three-dimensional stress state.
The results of Charpy tests performed on specimens made from
recrystallized tungsten plate material are clear: 0 J at 1000 °C
(1273 K). This result shows that for safety-relevant parts made of
tungsten plate material, recrystallization has to be avoided under
any circumstances.
Acknowledgments
This work, supported by the European Communities, was car-
ried out within the framework of the European Fusion Develop-
ment Agreement. The views and opinions expressed herein do
not necessarily reflect those of the European Commission.
The authors are grateful to our colleagues from PLANSEE Metall
GmbH, the University of Oxford, Department of Materials, and the
Karlsruhe Institute of Technology (KIT), Institute for Applied Mate-
rials (IAM), for their support and valuable contributions.
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