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Nuclear Materials and Energy 19 (2019) 184–188

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Nuclear Materials and Energy


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

Additive manufacturing of pure tungsten by means of selective laser beam T


melting with substrate preheating temperatures up to 1000 ∘C
A. v. Müllera,b, , G. Schlickc, R. Neua,b, C. Anstättc, T. Klimkaitd, J. Leed, B. Pascherd, M. Schmittc,

C. Seidelc
a
Max-Planck-Institut für Plasmaphysik, Garching, 85748 Germany
b
Technische Universität München, Garching, 85748 Germany
c
Fraunhofer IGCV, Augsburg, 86153 Germany
d
Aconity3D GmbH, Herzogenrath, 52134 Germany

ARTICLE INFO ABSTRACT

Keywords: The preferred plasma-facing material in present-day and future magnetic confinement thermonuclear fusion
Additive manufacturing devices is tungsten. This material is mainly chosen because of its high threshold energy for sputtering by hy-
Refractory metal drogen isotopes as well as its low retention of tritium within the material. From an engineering point of view,
Tungsten however, tungsten is a challenging material to work with as it is an inherently hard and brittle metal. In this
Laser beam melting
respect, established fabrication technologies for tungsten and tungsten based materials are a limiting factor
Plasma-facing material
directly affecting the design of plasma-facing components. Against this background, additive manufacturing
technologies could prove very beneficial with regard to plasma-facing component applications as they offer
flexibilities beyond the possibilities that conventional manufacturing methods offer. Within the present con-
tribution, we report on recent results regarding the additive manufacturing of tungsten by means of powder-bed
based selective laser beam melting. In more detail, investigations on pure tungsten manufactured by using
elevated substrate preheating temperatures up to 1000 ∘C are described.

1. Introduction material to work with as it is an inherently hard and brittle metal.


Established fabrication technologies for W are hence a limiting factor
Tungsten (W) is a refractory metal with outstanding properties. It for regarding the design and realisation of PFCs. Against this background,
example exhibits the highest melting point as well as the lowest vapour additive manufacturing (AM) technologies may prove useful as they offer
pressure of all metals [1]. Due to such exceptional properties, W and W flexibilities beyond the possibilities that conventional manufacturing
based alloys are typically used with respect to demanding high-tem- methods provide.
perature applications. One special area of application for W is as AM is a term that describes manufacturing processes in which three-
plasma-facing material (PFM) in present-day and future magnetic con- dimensional objects are created by means of sequential deposition of
finement thermonuclear fusion devices as for example in ASDEX Up- layers under computer control. Such processes offer advantages in
grade [2] or ITER [3]. For this application, W is mainly chosen as a comparison with conventional manufacturing technologies as parts
preferred PFM because of its high threshold energy for sputtering by with high geometrical complexity can be realised straightforwardly. In
hydrogen isotopes as well as its low retention of tritium within the the more recent past, substantial progress has been achieved regarding
material [4]. Apart from that, metallic composite materials that com- the AM of metals. In this respect, powder bed based laser beam melting
prise W as a reinforcing phase are becoming increasingly interesting (LBM) is a promising state-of-the-art technology which allows the direct
with regard to plasma-facing component (PFC) applications [5–8] both as AM of a wide variety of metals without the need for binder phases.
advanced plasma-facing and structural heat sink materials. With such Within such a process, powder material is selectively melted by means
composites improved material properties can be realised that enhance of a laser beam focused onto a powder bed. A comprehensive summary
the performance of PFCs which have to withstand severe particle, heat of this technology can for example be found in reference [9].
and neutron loads during operation. Within a previous study, AM of pure W was investigated by means
From an engineering point of view, however, W is a challenging of powder bed based LBM with substrate preheating temperatures of


Corresponding author at: Max-Planck-Institut für Plasmaphysik, Garching, 85748 Germany
E-mail address: alexander.v.mueller@ipp.mpg.de (A.v. Müller).

https://doi.org/10.1016/j.nme.2019.02.034
Received 13 August 2018; Received in revised form 5 February 2019; Accepted 24 February 2019
Available online 04 March 2019
2352-1791/ © 2019 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/BY-NC-ND/4.0/).
A.v. Müller, et al. Nuclear Materials and Energy 19 (2019) 184–188

200 ∘C. These studies showed that material samples with a high relative Table 2
mass density of approximately 98% could be consolidated directly by Investigated LBM process parameters in terms of substrate preheating, laser
means of LBM [10]. However, metallographic investigations revealed power and laser scanning speed.
that the material did exhibit pronounced microcracks. This behaviour Substrate preheating Laser power Laser scanning speed
was attributed to the intrinsic properties of W, especially its high duc-
tile-to-brittle transition temperature (DBTT), in combination with the high 600 ∘C 375 W 210 mm s−1 to 330 mm s−1
600 ∘C 400 W 330 mm s−1 to 510 mm s−1
thermal gradients that occur during an LBM process. In the literature, it
800 ∘C 375 W 210 mm s−1 to 330 mm s−1
is reported that LBM processing can induce spatial temperature gra- 800 ∘C 400 W 330 mm s−1 to 510 mm s−1
dients of approximately 102 K mm−1 to 104 K mm−1 as well as cooling 1000 ∘C 375 W 210 mm s−1 to 330 mm s−1
rates higher than 104 K s−1 [9]. To date, only a few papers regarding 1000 ∘C 400 W 300 mm s−1 to 840 mm s−1
AM of pure W can be found in the literature [11–16]. However, all these
investigations report that W is a specifically challenging material for
AM processes due to the intrinsic properties of this metal. In particular, strategy was fixed for all manufactured samples as 90 ∘ alternating bi-
Iveković et al. [14] reported that a substrate preheating of 400 ∘C is not directional. Moreover, the hatch spacing was held constant at 80 μm
sufficient in order to mitigate the formation of microcracks within the and the layer thickness was also fixed with 40 μm.
material during selective LBM processing.
Within this paper, we report on recent research activities regarding 3. Results and discussion
the AM of pure W by means of powder bed based LBM with substrate
preheating up to 1000 ∘C. In more detail, parametric studies regarding 3.1. Selective laser beam melting of cube-shaped tungsten samples
the consolidation of bulk material samples as well as the fabrication of
thin-walled W parts that were further processed to composite structures With the parameters mentioned in Section 2.3, cube-shaped samples
are described. with dimensions of 10 × 10 × 10 mm3 have been manufactured on
pure W substrate plates.
In Fig. 1, an image of such samples during the LBM process can be
2. Materials and methods
seen. The annealing colour of the consolidated material samples within
the powder-bed indicates their elevated temperature due to the fact that
2.1. Powder
they are directly built on and bonded to the preheated substrate plate.
In Fig. 2, an image of samples on a W substrate plate after manu-
In order to ensure good flowability of the powder during the AM
facturing and powder removal is shown. It is interesting to note that the
process spheroidised pure W powder (15 μm to 45 μm) was used in this
laser beam melted cube-shaped samples do exhibit rather clean surfaces
work. The results of the chemical analysis of the powder provided by
while the substrate plate seems to getter residual oxygen and undergo
the supplier are given in Table 1.
oxidation during the heating within the device chamber.

2.2. Laser beam melting facility


3.2. Mass density of cube-shaped tungsten samples
The manufacturing facility used within this work is an AconityONE,
Typically, an important prerequisite for acceptable thermo-
located at Aconity3D GmbH, Aachen, Germany. It is equipped with a
mechanical properties of a material is that it exhibits a sufficiently high
fibre laser operating at a wavelength of 1075 nm and an inductive
relative mass density and hence a low residual porosity after manu-
heating system which can raise the base plate temperature up to
facturing. That is the reason why this material parameter is commonly
1000 ∘C. In order to facilitate such high preheating temperatures a re-
used as an optimisation objective for AM processes. The mass density of
duced build platform with a diameter of 200 mm was used. Argon (Ar)
the W samples investigated within this work was determined by means
was used as protective gas. The laser was operated in focus (z = 0)
of densimetry based on Archimedes’ principle (density scale ABS 220-
while the focus diameter is approximately 100 μm. Movement of the
4N, Kern & Sohn GmbH). During the measurements, the samples were
laser spot is accomplished by a galvanometer scanner which alloaws the
immersed in ethanol (Ethanol absolute for analysis EMSURE ACS, ISO,
device to reach scanning speeds of up to 10 m s−1.

2.3. Investigated parameter space for cube-shaped tungsten samples

The selection of the process parameters investigated within this


work was based on experience gained during previous studies [10]. In
terms of substrate preheating, the process was investigated for pre-
heating temperatures of 600 ∘C, 800 ∘C and 1000 ∘C. The investigated
LBM process parameters in terms of laser power, laser scanning speed
and substrate preheating are summarised in Table 2. The laser scanning

Table 1
Chemical composition of the used W powder.
Element wt.%

W ‐ tungsten ≥ 99.9
Cr ‐ chromium < 0.001
Fe ‐ iron ≤ 0.001
Mo ‐ molybdenum ≤ 0.003
Ni ‐ nickel < 0.001 Fig. 1. W samples during the LBM process within the powder bed; the an-
O ‐ oxygen ≤ 0.03 nealing colour of the consolidated material samples indicates their elevated
Ta ‐ tantalum < 0.001
temperature; the greenish colour of the image is due to the laser protection
Others ≤ 0.002
glass.

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A.v. Müller, et al. Nuclear Materials and Energy 19 (2019) 184–188

Fig. 2. Typical cube-shaped W samples with an edge length of 10 mm on W


substrate plate after the LBM process and powder removal.

Reag Ph Eur., Merck KGaA) at room temperature.


The relative mass densities of the W samples produced within this
work are illustrated in Fig. 3 where the density of the samples versus
the applied energy density is shown. The illustration includes data of
samples manufactured with different substrate preheating temperatures
(600 ∘C, 800 ∘C, 1000 ∘C) as well as different laser powers (375 W,
400 W). The energy density illustrated in Fig. 3 is calculated according
to

P
E =
vst (1)

with the laser power P, the laser scanning speed v, the hatch spacing s as
well as the layer thickness t. Apart from the fact that Fig. 3 confirms
that W can be consolidated reasonably by means of powder bed based
LBM several observations can be made in addition. On the one hand, it
can be seen that there is a general trend of increasing mass density of
the samples with increasing substrate preheating temperature. In this
sense, it can be concluded that increased substrate preheating tem-
peratures are in general beneficial for LBM processing of pure W. On the
other hand, it can be seen that for the investigated parameters energy
densities of approximately 300 J mm−3 and higher are not suitable as
such parameters lead to decreased densification of the material. Fur-
thermore, it can be seen that the highest investigated preheating tem-
perature of 1000 ∘C in combination with the high laser power of 400 W

Fig. 4. Optical microsections perpendicular to building direction of LBM W


samples manufactured with a substrate preheating of 1000 ∘C and a laser power
of 400 W; (a) laser scanning speed of 300 mm s−1, (b) laser scanning speed of
510 mm s−1 and (c) laser scanning speed of 840 mm s−1.

tend to result in the highest measured relative mass densities of the


samples. As these two main process parameters have been regarded as
most suited for the LBM of pure W the corresponding parameter space
has been investigated down to energy densities of approximately
150 J mm−3. However, the data indicates that there is again a trend of
slightly decreasing mass density for decreasing energy densities below
approximately 200 J mm−3. This resembles a typical behaviour en-
Fig. 3. Relative mass density of the manufactured W samples versus applied countered with respect to material processing by means of selective
energy density; the illustration includes data of samples manufactured with LBM which is characterised by a certain processing window that com-
different substrate preheating temperatures (600 ∘C, 800 ∘C, 1000 ∘C) as well as prises manufacturing parameters yielding a high densification of the
different laser powers (375 W, 400 W). laser beam melted material. Usually, too low energy densities lead to

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A.v. Müller, et al. Nuclear Materials and Energy 19 (2019) 184–188

interrupted melting tracks that in turn imply porosity while excessive


energy densities result in deep melting tracks with keyhole porosity
formation [9].

3.3. Microstructure of cube-shaped tungsten samples

Within this section, exemplary microsections of the additively


manufactured W samples are shown. The illustrated metallographic
cross sections are all prepared perpendicular to the building direction of
the samples. In Fig. 4, three samples are illustrated that were produced
with a substrate preheating of 1000 ∘C and a laser power of 400 W. For
these two parameters, the boundaries of the investigated parameter
space as well as a reasonable choice in terms of laser scanning speed are
shown. In Fig. 4a, a sample manufactured with a laser scanning speed of
300 mm s−1, corresponding to an energy density of ca. 420 J mm 3, is
illustrated. It can be seen that the sample exhibits macroscopic defects
especially plainly visible porosity. In Fig. 4b, a sample manufactured
with a higher laser scanning speed of 510 mm s−1, i.e. a lower energy
density, is shown. It can be seen that the sample exhibits clearly less
porosity, compared with the sample shown in Fig. 4a, as is also con-
firmed by Archimedes’ densimetry. In Fig. 4c, a sample manufactured
with a laser scanning speed of 840 mm s−1, i.e. the highest laser
scanning speed investigated within this work, is shown. It can be seen
that the sample exhibits again slightly more porosity, compared with
the sample shown in Fig. 4b, which is also confirmed by Archimedes’
densimetry. One of the aims of the present study is to investigate the
potentially positive influence of an elevated substrate preheating tem-
perature during the LBM process as it is well-known that W as a body-
centred cubic metal exhibits a rather high DBTT. Hence, microsections
are shown in Fig. 5 for samples manufactured with similar parameters
but with different substrate preheating temperatures. Fig. 5a is taken
from a previous study [10] and shows a sample that has been manu-
factured with a substrate preheating of 200 ∘C while in Fig. 5b a sample
is shown that has been manufactured with a substrate preheating of

Fig. 6. (a) W honeycomb structures on W substrate plate and (b) top view of W
honeycomb structure manufactured by means of selective LBM.

1000 ∘C. The cross sections illustrated in Fig. 5 indicate that the mi-
crocrack formation is to some extent mitigated and crack density is
reduced due to the substrate preheating but it is not completely in-
hibited. Furthermore, it can be seen that the cracking morphology is
somewhat different. In Fig. 5a, the cracks form a network that can di-
rectly be attributed to the scan tracks of the laser beam while this is not
apparently visible for the sample shown in Fig. 5b, manufactured with a
substrate preheating of 1000 ∘C. Overall, it can be summarised from the
microscopic investigations that pure W fabricated by means of LBM can
exhibit reasonable densification but that the material does also exhibit
defects which are typical for selective LBM, like porosity and cracking.
An elevated substrate preheating temperature during LBM of up to
1000 ∘C seems to have a positive influence regarding the crack forma-
tion but does not mitigate the formation of crack defects completely. It
can hence be concluded that the fabrication of defect free W through
selective LBM is still a rather challenging task.

4. Additively manufactured tungsten honeycomb structures

Fig. 5. Optical microsections perpendicular to building direction of LBM W As has been mentioned within the introductory section, one of the
samples manufactured with a substrate preheating of (a) 200 ∘C (laser power main advantages of AM technologies is that with such a process parts
400 W, laser scanning speed 500 mm s−1) [10] and (b) 1000 ∘C (laser power with almost any shape or geometry can be realised very flexibly by
400 W, laser scanning speed 510 mm s−1). means of layerwise deposition of material. In order to demonstrate

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A.v. Müller, et al. Nuclear Materials and Energy 19 (2019) 184–188

temperatures are beneficial for material consolidation during LBM. It


has been shown that material fabricated with a substrate preheating of
1000 ∘C exhibits a potentially lower crack density although there is no
complete mitigation of the microcrack formation even at such elevated
process temperatures.
Within the investigated parameter space, reasonable manufacturing
parameters have been identified with a deposited energy density of
approximately 250 J mm−3 for a laser power of 400 W.
Apart from that, it has been demonstrated that thin-walled W parts
can be produced straightforwardly by means of powder-bed based LBM.
Such W structures could be beneficial for various applications but
especially with respect to the manufacturing of tailored composite
structures as has been shown for a W–Cu honeycomb composite.

Conflict of interest

The authors declare that they have no known competing financial


interests or personal relationships that could have appeared to influ-
Fig. 7. Microsection of a W-Cu composite based on an additively manufactured ence the work reported in this paper.
W honeycomb structure and fabricated by means of liquid Cu infiltration.
Acknowledgement
these possibilities thin-walled W honeycomb structures have been
manufactured directly by means of the investigated LBM process. An This work has been carried out within the framework of the
image of such W honeycombs is illustrated in Fig. 6a. In Fig. 6b, a EUROfusion Consortium and has received funding from the Euratom
microscopic top view of the W honeycomb structure is illustrated. The research and training programme 2014–2018 under grant agreement
struts of the W honeycomb structures shown in Fig. 6 correspond to one No 633053. The views and opinions expressed herein do not necessarily
single laser melting track. Furthermore, it should be mentioned that the reflect those of the European Commission. Furthermore, the authors
issues with residual stresses and the corresponding microcrack forma- want to acknowledge support by Mrs. K. Hunger and Dr. M. Balden with
tion as described within the previous section for bulk material are ex- metallographical and microscopic investigations.
pected to be less problematic for thin-walled structures as shown in
Fig. 6. References

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