Selective Laser Melting of Tungsten-Copper Functionally Graded Material - Chaolin - 2019

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Materials Letters 237 (2019) 328–331

Contents lists available at ScienceDirect

Materials Letters
journal homepage: www.elsevier.com/locate/mlblue

Selective laser melting of tungsten-copper functionally graded material


Chaolin Tan a,b,⇑, Kesong Zhou a,b,⇑, Tongchun Kuang a
a
School of Materials Science and Engineering, South China University of Technology, Guangzhou 510640, China
b
Guangdong Institute of New Materials, Guangzhou 510651, China

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

Article history: A tungsten-copper functionally graded material was processed based on SLM additive manufacture
Received 5 October 2018 despite encountering some difficulties from materials characters. The effect of laser parameter on the
Received in revised form 5 November 2018 interfacial defects and bonding performance are evaluated. The SLM produced tungsten is in columnar
Accepted 24 November 2018
structures with random orientation. Plenty of fine tungsten grains are present at the bonding region,
Available online 27 November 2018
owing to a high cooling rate incited by the underlying copper. A metallurgically bonded interface with
a 50–80 lm inter-diffusion region is formed. The interfacial bonding mechanism, which associates with
Keywords:
intense Marangoni convection at the interface, is revealed and discussed.
Selective laser melting
Powder technology
Ó 2018 Elsevier B.V. All rights reserved.
FGM
Tungsten
Nuclear materials
W-Cu

1. Introduction able relative density of 98.5% [3]. Besides, high production flexibil-
ity of SLM, derived from incremental layer-wise deposition
Plasma-facing components (PFC), which are indispensable to manner, provides unique advantages of producing complex-
fusion reactors such as the ITER and DEMO, consist of plasma fac- shaped W-Cu FGM. Moreover, SLM process of FGM components
ing materials (PFM) and heat sink materials [1]. Tungsten-copper could obtain a lower interfacial residual stress and a higher bond-
(W-Cu) functionally graded material (FGM) is a typical and ing strength than laser/arc welding [6]. However, there are also
widely-used PFC, since W is a promising PFM material due to its some intractable issues in SLM W-Cu FGM, which originate from
inherent high melting temperature, low erosion rate under plasma the mutual effects between matter and laser:
loading, limited tritium retention, etc. [2,3]; and copper is an ideal
heat-sink material due to the high thermal conductivity. However, (i) SLM of pure W encounters many intractable defects such as
the inherently large differences of physical and chemical character- balling, cracking and lack of fusion, which associate with the
istics between W and Cu make W-Cu FGM difficult to be processed intrinsic high surface tension and viscosity, high brittleness
by traditional fabrication techniques, such as powder- and oxidation sensitivity, high melting point and thermal
metallurgical sintering, plasma spraying, infiltration welding, etc. conductivity of W, respectively[3,7].
[1,4,5]. For instance, the large melting point differences, mutual (ii) The high thermal conductivity and low laser energy absorp-
insolubility and the high contact angle of these two metals lead tion (<5%) of bulk Cu cut down the temperature of melt pool
to difficulties in conventional sintering methods [1]. Besides, rapidly, which makes the high melting point W hard to be
plasma spraying of W-Cu FGM faces with the problems of limited melted and deposited on the Cu.
thickness, low interfacial bonding strength and the high porosity of (iii) No intermetallic phase alongside with mutual insolubility
the coating [5]. between W and Cu, suggesting a limited bonding strength.
Selective laser melting (SLM) additive manufacturing is capable Worsely, significant different thermal expansion coefficients
of melting and consolidating refractory metal powder by using a and rapid cooling rate could cause large misfit strain and
high-energy density laser beam. Former research has proved SLM residual stress at the interface, which further impair the
could produce pure tungsten with a high strength and an achiev- interfacial bonding.
In this work, a W-Cu FGM was firstly produced by SLM based
⇑ Corresponding authors at: School of Materials Science and Engineering, South hybrid manufacture. The effects of laser parameter on the interfa-
China University of Technology, Guangzhou 510640, China. cial defects, microstructure and bonding strength, were discussed.
E-mail addresses: tclscut@163.com (C. Tan), kszhou2004@163.com (K. Zhou). Moreover, interfacial bonding mechanism was also elucidated.

https://doi.org/10.1016/j.matlet.2018.11.127
0167-577X/Ó 2018 Elsevier B.V. All rights reserved.
C. Tan et al. / Materials Letters 237 (2019) 328–331 329

2. Experimental details stresses accumulated from SLM processes which follow the ther-
mal gradient mechanism [8]. Second, the significant differences
A plasma spheroidized pure tungsten powder (mean diameter, of thermal expansion coefficient and thermal conductivity
17 lm) supplied by Tekna Advanced Materials Inc. was used for between Cu and W inevitably caused large misfit strain and resid-
SLM processes. The experiments were fulfilled in an EOS M290 ual stresses in the interface, which also leads to solidification
SLM system. As illustrated in Fig. 1a, a computer numerical control cracks [3].
machined bulk T2 copper was sand-blasted and fixed on the sub- Interfacial EBSD analysis of the g2 specimen is provided in
strate, and then the tungsten powder was deposited on Cu by Fig. 2. The inverse pole figure reveals a columnar W structures with
SLM. Based on our former work about parameters optimisation random orientation in Fig. 2a. The small maximum intensity value
in SLM pure tungsten [3], four linear energies (g, defined as (about 3.1) of the corresponding pole figures (PF) in Fig. 2b also
g = laser power/scan speed), were assigned for the SLM processes demonstrated an absence of strong textures. Besides, the highest
including 0.50 J/mm (g1), 0.68 J/mm (g2), 0.75 J/mm (g3) and intensity planes in these three PFs are different, the highest inten-
1.25 J/mm (g4). A layer thickness of 20 lm was selected, and the sity in {0 0 1} PF is close to h0 1 1i directions, while it in {1 1 1} and
laser scanned in a zigzag raster pattern with 67° inter-layer {1 1 0} PFs are close to h0 0 1i directions, which indicates a random
rotation. crystallographic orientation was detected. Normally, the h1 0 0i
The interfacial defects and microstructures were observed by a crystallographic orientation is the preferable crystallisation direc-
Zeiss Merlin field emission scanning electron microscope (FE-SEM). tion for cubic crystal alloys during a laser melt pool solidification
The interfacial electron back-scattered diffraction (EBSD) test was [9]. The non-textured microstructures are presumably caused by
carried out through an EDAX Hikari EBSD detector on an FEI Nova the 67° rotations among layers, which suppressed temperature
NanoSEM 450 SEM system, using a step size of 0.8 lm at 20 kV. gradient and undercooling degree by altering of heat flux direction
Phase compositions were detected by X-ray diffraction (XRD) in a [10]. The grain boundary map Fig. 2c reveals a gradient size distri-
Bruker D8 advance diffractometer system using a Cu Ka radiation bution of tungsten grains at the interface. Fine grains at the bond-
(0.15418 nm) operated at 40 kV and 40 mA with a step size of ing region could be incited by the high thermal conductive Cu
0.02°. The flexural specimen, with Cu-W interface in the central (401 Wm1 k1). The effect of Cu was gradually reduced with lay-
X-Z plane, was 3  4  25 mm in size after grinding. The flexural ers increase, so larger W grains were present above the bonding
tests were carried out on a CMT4204 universal material testing region. The W grains with 2–5° boundary angle distribute mainly
machine using a loading speed of 0.25 mm/min. at the interface, while the high-angle grain boundaries (HAGBs,
15°) are more predominant (about 73% in fraction) in the whole
3. Results and discussion W. HAGBs are more disordered, with large misfit areas and high
density of dislocations, which could be caused by high interfacial
Fig. 1b-e reveals the effect of g on the interfacial defects of the residual stress due to the high cooling rate and significant differ-
SLM-produced W-Cu FGM samples. The large irregular-shaped ences of thermal expansion coefficients (a, aCu  4aW). The grain
pores within some un-melted powder particles in the g1 sample size distribution of W accounted from Fig. 2c is outlined in
(Fig. 1b) are typical characters of lacking fusion due to insufficient Fig. 2d, the average grain size is about 14 lm, which is much smal-
energy input, which could be caused by low laser energy absorp- ler than grains of commercial pure W (about 40 lm)[11], and tra-
tion and rapid heat dissipation of underlying Cu. In contrast, pores ditionally CVD deposited W (up to 50 lm) on Cu [12].
in Fig. 1c-e are reduced owing to the increased g. The g2 and g4 Fig. 3a shows the XRD analyses of initial W powder, bulk Cu and
samples exhibit fewer pore defects, but the cracks seem to be more the W-Cu FGM interface, which reveals no intermetallic phase
pronounced. The cracks origin from two aspects: first, residual exists between W and Cu. Interestingly, an interfacial W-Cu

Fig. 1. (a) Schematic diagram of SLM manufacture of W-Cu FGM; (b)-(e) interfacial SEM observations of different g processed W-Cu FGM samples.
330 C. Tan et al. / Materials Letters 237 (2019) 328–331

Fig. 2. Interfacial EBSD analysis of SLM-produced g2 specimen: (a) Color inverse pole figure showing grain orientation distributions, (b) pole figure showing random texture,
(c) grain boundary map, and (d) grain size distributions of tungsten. (For interpretation of the references to colour in this figure legend, the reader is referred to the web
version of this article.)

Fig. 3. (a) XRD patterns taken from tungsten powder, bulk Cu and W-Cu interface, (b) SEM morphology showing an inter-diffusion W-Cu interface, and (c) schematics of W-
Cu interfacial bonding mechanism.

bonding with the inter-diffusion region of 50–80 lm is present in effect, which causes mass transfer between two fluids interface
Fig. 3b, which probably accounts for the bonding between W and due to the surface tension (r) gradient. Increasing of r or/and
Cu. This inter-diffusion region is likely caused by the Marangoni temperature gradient (DT) can enhance the thermal Marangoni
C. Tan et al. / Materials Letters 237 (2019) 328–331 331

Fig. 4. (a) Flexural stress-strain curves, and (d) lateral view of W-Cu samples after fracture.

convection DM [13]. As illustrated in Fig. 3c, the temperature of the 4. Conclusions


central melt pool (A) is higher than the boundaries (B and C), i.e.,
TA > TB and TA > TC, then rA < rB and rA < rC. A high r liquid pulls In summary, a W-Cu FGM was fulfilled based on SLM additive
on the surrounding liquid more strongly than one with a lower r. manufacture. Irregular-shaped pores and cracks were the main
In this case, the gradient surface tension caused the liquid to flow defects at the interface due to the intrinsic properties of materials.
away from the central melt pool to the boundary [14]. Besides, the The SLM produced W had 14 lm average sized columnar struc-
DT of melt pool was enhanced by the underlying high thermal con- tures with random orientation. The W-Cu composite bonding
ductive copper, so the Marangoni convection at the W-Cu interface region reached up to 80 lm owing to the intense Marangoni con-
would be more intense [6]. The sunken spherical W particles into vection at the interface enhanced by the high thermal conductive
the Cu are caused by gravity. Because, on the basis of a large gap Cu. Both the interfacial microstructures and flexural tests revealed
(2337 °C) of melting point between Cu and W, the underlying Cu that the 0.68 J/mm parameter was superior to others. This work
could be preferentially melted as a liquid by the laser penetration suggested novel approaches to produce refractory metals and its
and the rapid heat dissipation from the W melt pool. So none fully FGM by SLM additive manufacture or SLM based hybrid processes.
melted heavy W particles fell into the liquid Cu under gravity.
Consequently, a high thickness W-Cu composite bonding region Acknowledgements
was achieved.
A three-point bending test was adopted to test the mechanical This work was financially supported by Guangdong Academy of
properties, as well as to evaluate the bonding strength, since shear Science Projects (2018GDASCX-0402, 2017GDASCX-0202,
stress presents at the W-Cu interface during bending owing to 2017GDASCX-0111, 2018GDASCX-0111).
the pronounced differences in plasticity and Young’s modulus
(E, EW  5ECu). The results of bending tests in Fig. 4a prove that References
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