Fusion Engineering and Design 86 (2011) 25852588

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Fusion Engineering and Design
j our nal homepage: www. el sevi er . com/ l ocat e/ f usengdes
Investigation of tungsten/EUROFER97 diffusion bonding using Nb interlayer
W.W. Basuki

, J. Aktaa
Karlsruhe Institute of Technology (KIT), Institute for Applied Materials (IAM), Hermann-von-Helmholtz-Platz 1, D-76344 Eggenstein-Leopoldshafen, Germany
a r t i c l e i n f o
Article history:
Available online 27 March 2011
Keywords:
Fusion
Joining
Diffusion bonding
EUROFER
Tungsten
Niobium
a b s t r a c t
Diffusion boning is a preferred method to join tungsten and EUROFER97 for the manufacturing of some
components in the fusion technology. To reduce the interfacial residual stresses induced during the dif-
fusion bonding by the large mismatch of their coefcients of thermal expansion, a Nb plate is introduced
as an interlayer. The diffusion bonding experiment was conducted for 1h at 1050

C and with a pres-

sure which yield at the EUROFER97 side to a calculated creep strain of 8%. Investigations of the bonded
specimens show a hard reaction layer consisted of niobium carbides (Nb
2
C and Nb
6
C
5
) at the interface
between EUROFER97 and Nb, which can weaken the bonding interface especially at RT. At a testing tem-
perature of 550

C, the strength of the bonded specimens is improved and close to that of EUROFER97.
An improvement in toughness is also observed by means of Charpy impact tests.
2011 Elsevier B.V. All rights reserved.
1. Introduction
The divertor of fusion power plants is exposed to high energetic
particles resulting fromthe fusionreactions. Due to the highkinetic
energy, the surface of plasma facing material will be subjected
to a high heat load and to physical and chemical sputtering pro-
cesses. Tungsten as a lowactivation, refractory and high Z material
is selected to handle the problems in the DEMO (DEMOnstration)
fusion power plant [1,2].
In the helium cooled divertor, which should withstand a heat
ux up to 15MW/m
2
, tungsten shall be used as a shield as well
as a structural material. Its use as a structural material however is
limited to the high temperature parts which shall be connected to
the low temperature parts built from the reduced activation fer-
ritic/martensitic steel EUROFER97. The method for realizing such
kind of connection is restricted by a lot of problems related to
the large differences in the physical properties of both materials.
For instance, the large differences of their melting temperature
(3422

C for tungsten and 1536

C for steel depending on the

alloying elements) make themnot possible tobe joinedbymeans of
a conventional fusionwelding technique. The most important issue
by connecting both materials especially at elevated temperature is
the large mismatch of their CTE (coefcient of thermal expansion,
4.510
6
K
1
for tungsten and 12.710
6
K
1
for EUROFER97
[3]). It causes high thermally induced residual stresses at the inter-
face, when the connected materials are cooled down from the
bonding temperature to RT (room temperature). This results in a
reduction in tensile strength and toughness of the joint.

Corresponding author. Tel.: +49 721 608 22946; fax: +49 721 608 24566.
E-mail address: Widodo.Basuki@kit.edu (W.W. Basuki).
Until now several techniques including brazing and solid state
diffusion bonding have been investigated to join tungsten with
steel. The suitable brazing materials result in brittle brazing lay-
ers and thus a joint with a very lowtoughness [4]. In addition, they
need a process temperature usually much higher than the recrys-
tallisation temperature of the materials to be joined [4,5]. To avoid
a substantial change in the microstructure and properties of the
materials to be joined, the solid state diffusion bonding is consid-
ered. Diffusion bonding experiments have been performed to join
tungsten to RAFM steel directly [6,7]. The results showed a thin
brittle intermetallic phase, which had a very high tensile strength
(e.g. 440MPa at 650

C) [7]. Unfortunately, the bonding seam was

not able to endure the thermal loading due to the large CTE mis-
match of the bulk materials and therefore failed during PBHT (post
bonding heat treatment), which is necessary to recover the prop-
erties of steel. To solve this problem, an Nb interlayer with a CTE in
the range between the CTE of tungsten and EUROFER97 has been
used and investigated in this work.
2. Experimental procedures
The bulk materials used in this work were an 18mm diameter
polycrystalline tungsten rod with a purity of 99.96% manufactured
by Plansee Metall GmbH and a 25mm thick EUROFER97 plate
(2nd batch with a heat number of 993402) ordered from Ger-
man manufacturer Saarschmiede. The main alloying elements in
EUROFER97 were Fe (bal.), Cr (8.59.5wt.%), W(1.01.2wt.%) with
C (0.1wt.%) [8]. The commercial Nb plate used as interlayer had
a thickness of 1mm with a purity of 99.9% and was delivered in
annealed condition. As bonding specimens, tungsten-rod was cut
by EDM (Electrical Discharge Machining) in a length of 16mm,
0920-3796/$ see front matter 2011 Elsevier B.V. All rights reserved.
doi:10.1016/j.fusengdes.2011.03.017
2586 W.W. Basuki, J. Aktaa / Fusion Engineering and Design 86 (2011) 25852588
EUROFER97-plate in a diameter of 18mm and a length of 22mm
with a bonding surface parallel to the rolling plane. The Nb inter-
layer was cut to a disc with a diameter of 18mm.
Prior to diffusion bonding, the bonding surfaces of all materials
were ground with SiC emery paper and polished using diamond
suspensionupto a surface roughness R
t
of about 0.2m. Thereafter
the specimens were cleaned two times (each time for 15min) in an
ultrasonic bath using acetone at a bath temperature of 35

C and
then piled up with the Nb interlayer inserted between tungsten
and EUROFER97 and then placed in the middle of the compression
plate in the bonding chamber.
The diffusion bonding processes were performed in a vacuum
atmosphere of about 6.010
5
mbar and at 1050

C, at which
the recrystallisation of EUROFER97 [8] begins. The uniaxial bond-
ing pressure was determined, in a way that the creep strain on
EUROFER97 side after 1h was about 8%. To calculate the creep
deformation of EUROFER97, the parameters of Norton power creep
law were used [7]. After the bonding process the bonded sample
was relieved and cooled down to 200

C. Subsequently, the PBHT

was done at 760

C for 90min, and then cooled down to RT.

After diffusion bonding, the microstructure and the chemical
composition along the bonding seams were analyzed using SEM
(scanning electron microscope) and AES (Auger electron spec-
troscopy). The reaction phases were conrmed by XRD (X-ray
diffraction). For investigationof thetensileproperties of thebonded
specimens, cylindrical tensile specimens with a diameter of 2mm
and gauge length of 7mm were used. The investigation was con-
ducted at a constant displacement rate of 0.07mm/s. The fracture
surfaces were revealed using SEM equipped with EDX (energy dis-
persive X-ray spectroscopy). The toughness at the bonding seams
was examined by means of Charpy impact tests using miniatur-
ized KLST Charpy specimens [9]. The equipment is full automated
with maximum impact energy of 25kJ. The hardness of the possi-
ble formed intermetallic layer was measured using a nanoindenter
with a Berkovich-tip. The measurements were done with a strain
rate of 0.05s
1
and an indentation depth limit of 500nm.
3. Results and discussion
After diffusion bonding, it is evident, that the inelastic deforma-
tion takes place on the EUROFER97 side only. Regarding the initial
length of EUROFER97, this is about 8%.
The microstructures at the interfaces of diffusion bonded spec-
imen are presented in Fig. 1. The SEM photomicrographs show
clearly, that no micro-cracks are observed along and perpendicu-
lar to the bonding interfaces of EUROFER97/Nb (Fig. 1a) and Nb/W
(Fig. 1b). It seems that the Nb interlayer can reduce the residual
stress caused by the CTE mismatch of tungsten and EUROFER97
and improve the bonding even PBHT was performed. The charac-
teristic beads structures are not found along the bonding interface,
which indicates that the pores formed by surface roughness pro-
les of materials to be bonded are lled and closured completely by
means of various diffusion mechanisms during diffusion bonding
processes. In the case of diffusion bonding of dissimilar materials,
the diffusion processes at elevated temperature do not just ll up
the pores but also provide interdiffusion of atoms across the bond-
ing interfaces simultaneously causing the formation of diffusion
layers. The layers are usually thin depending on the materials to be
bonded, bonding temperature and bonding duration. Fig. 1a shows
such kind of diffusion layer at the interface of EUROFER97/Nb with
a thickness of 78m. A thinner layer with a thickness of 12m
can be found at the interface of Nb/W in Fig. 1b.
To investigate the elemental composition and its distribution in
the layers, elemental concentration proles were measured across
each layer by means of AES. The results are presented in Fig. 2a for
Fig. 1. SEM photomicrographs at bonding interfaces between (a) EUROFER97 and
Nb interlayer, (b) Nb interlayer and W.
EUROFER97/Nb and in Fig. 2b for Nb/W. At the EUROFER97 side in
Fig. 2a, the alteration of C concentration cannot be measured accu-
rately due toits lowcontent inEUROFER97. At the other side, a peak
of C at a position of 40m is supposed to be an impurity in some
places in the Nb interlayer. The diffusion layer shown in Fig. 1a can
be found in Fig. 2a in the range between 27mand 35m. Accord-
ing to Fe mapping on this layer, the Fe atoms are found to diffuse
through the interface and occupy the dislocations in this layer. The
atomic concentration of C increases up to about 50at.% and has
a similar distribution as well as Nb. This high C concentration is
caused by decarburization of the martensitic phase of EUROFER97.
0 5 10 15 20 25 30 35 40 45
Distance (m)
O
Fe
Cr
Nb
C
0
20
40
60
80
100 )
%
(
n
o
i
t
a
r
t
n
e
c
n
o
C
c
i
m
o
t
A
50
a)
Nb
W
C
O
b)
0 1 2 3 4 5 6 7 8 9
Distance (m)
0
20
40
60
80
100 )
%
(
n
o
i
t
a
r
t
n
e
c
n
o
C
c
i
m
o
t
A
10
Fig. 2. AES analysis of element concentration across the interfaces between (a)
EUROFER97 and Nb interlayer, (b) Nb interlayer and W.
W.W. Basuki, J. Aktaa / Fusion Engineering and Design 86 (2011) 25852588 2587

30 40 50 60 70
2 (deg.)
)
.
u
.
a
(
y
t
i
s
n
e
t
n
I
EUROFER97 side
r
C
-
e
F
b
N
Nb side
C
b
N
C
b
N
C
b
N
C
b
N
b
N
Fig. 3. XRD investigation on the fractured surfaces of a tensile specimen tested at
RT.
Fig. 4. Microstructure at the interface between EUROFER97 and Nb interlayer.
The AES spectrumof C in the kinetic energy range between 240 and
300eV shows the typical spectrum of carbide in this area. Accord-
ing to the XRD investigation on the fractured surfaces of a tensile
specimen both at the EUROFER97 side and Nb side, the carbides as
showninFig. 3 consist of Nb
2
Cand Nb
6
C
5
. This regionis considered
as a reactionlayer. Concerning the decarburization, the microstruc-
ture closed to the reaction layer on the EUROFER97 side, as shown
in Fig. 4, is expected to be a ferritic phase.
Other than EUROFER97/Nb, the distribution curves in Fig. 2b
show a stepless change of element concentration at the interface
of Nb/W, which indicates that neither intermetallic phases nor
other reaction compounds are found in this region. Furthermore,
the peak of the C concentration in the Nb interlayer might be par-
ticle impurities caused by the grinding and polishing. According to
the elemental mapping, the impurity particles emerge extremely
seldom in some places on the surface.
Based on the microstructure investigations, the hardness across
the reactionlayer betweenEUROFER97andNbinterlayer was mea-
sured by means of nanoindentation. The results are presented in
Fig. 5. As expected, the niobium carbide layer possesses a highest
hardness of about 5.5GPa. On the EUROFER97 side, the hardness
in the ferritic phase drops drastically down to about 2.6GPa and
then increase to 3.3GPa, which is comparable with the hardness of
EUROFER97 in the as-delivered condition, which however deviates
from 2.95GPa to 3.40GPa.
-80 -40 0 40 80
Distance from interface ( m)
0
1
2
3
4
5
6
)
a
P
G
(
s
s
e
n
d
r
a
H
r
e
y
a
l
n
o
i
t
c
a
e
R
Nb - interlayer EUROFER97
Fig. 5. Hardness distribution across the reaction layer.
Fig. 6. SEM photomicrograph of the fracture surface on the EUROFER97 side of
diffusion bonded specimen, tensile tested at RT.
Others mechanical properties of bonded specimens resulted
from Charpy impact testing and tensile testing are presented in
Table 1. The base material properties of EUROFER97 and tungsten
with the similar testing temperature are also summarized in the
table for comparison. According to the values of Charpy impact
toughness a
v
, the diffusion bonded samples at RT have toughness
values close to tungsten. Heating to 550

C improves the impact

toughness of the bonded specimen by about 42%. However, in rela-
tion to the value of tungsten at the same temperature, this value
seems to be too low. The brittleness of the specimen is caused by
the hard carbide layer as discussed before.
In the case of tensile tests at RT, the bonded specimen possesses
a relatively high strength. Compared to EUROFER97, the tensile
strength
UTS
just reaches about 41% of that of EUROFER97. But the

UTS
of Nb in the annealed condition is essentially much lower than
EUROFER97. For instance, the
UTS
of thick wire of Nb in annealed
condition is just about 300MPa [10] or about 10% higher than the

UTS
of the bonded specimen. The specimen is fractured at EURO-
FER97/Nb interface without any plastic deformation. The fracture
surface of the specimen on the EUROFER97 side is given in Fig. 6.
The atomic concentration of Fe in region Ais up to 25%. In region
B, the transcrystalline brittle failure is evident by the present of the
river patternonthe fracture surfaces. The element measuredinthis
region is Nb.
At a testing temperature of 550

C,
UTS
increases and reaches
87% of
UTS
of EUROFER97. The bonded specimen deforms
Table 1
Mechanical properties of diffusion bonded specimens and the bulk materials in as-obtained condition.
RT 550

C
Joint W EUROFER97 [8] Joint W EUROFER97 [8]
av (J/cm
2
) 1.50 1.66 107 2.13 6.70

UTS
(MPa) 272 1260 663 299 428 345

y,0.2
(MPa) 1252 544 290 399 322
A (%) 0.41 24.80 0.82 29.08 21.55
Note: Italics signify mechanical properties of one of the parent materials, which are reasonable for comparison with those of the bonded specimens.
2588 W.W. Basuki, J. Aktaa / Fusion Engineering and Design 86 (2011) 25852588
Fig. 7. SEMphotomicrographof thefracturesurfaceonthetungstensideof diffusion
bonded specimen, tensile tested at 550

C.
plastically. The relation between the 0.2% offset yield strength

y,0.2
of bonded specimen and bulk materials indicates that plastic
deformation takes place just local in the Nb interlayer. Before the
bonded specimen fails at Nb/W interface, the uniform elongation
is obtained. The strain to rupture A as listed in Table 1 is related
to the 7mm gauge length and therefore seem to be too low. The
evident of ductility can be found on the fracture surface in Fig. 7,
in which cup-like structures in region A are observed. The main
constituent elements in this region are Nb and W. The fracture sur-
face analysis reveals also some island-like regions (such as region
B), which indicate not properly bonded areas. The crack along the
grain boundaries of tungsten shown by the black arrowpropagates
but does not widen in this region.
4. Conclusions
Diffusion bonding of tungsten and EUROFER97 using Nb
interlayer with PBHT was successfully conducted. The bonding
interfaces are sound. A hard and brittle reaction layer consisted of
niobium carbides are found at the interface between EUROFER97
and Nb. The bonded specimens are able to endure a high tensile
stress especially at 550

C. Its tensile strength at this temperature

is even close to that of EUROFER97. However, the Charpy impact
toughness is still lower than that of tungsten. The surface frac-
ture analyses on the tensile specimens tested at RT reveal a brittle
fracture in the reaction layer. At testing temperature of 550

C, the
fracture occurs at the interface of Nb/W. Aductile fracture indicated
by the cup-like structures is observed at the fracture surface on the
tungsten side. Unfortunately, few of small island-like areas, which
are not properly bonded, are found.
Acknowledgements
This work, supported by the European Communities under the
contract of association between EURATOM and Karlsruhe Insti-
tute of Technology, was carried out within the framework of the
European Fusion Development Agreement. The views and opinions
expressed herein do not necessarily reect those of the European
Commission. The authors are indebted to Mr. T. Weingrtner for
the AES analysis and Mrs. C. Odemer for the XRD investigation.
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