You are on page 1of 11

Materials Characterization 167 (2020) 110489

Contents lists available at ScienceDirect

Materials Characterization
journal homepage: www.elsevier.com/locate/matchar

Dual interfacial characterization and property in multi-material selective T


laser melting of 316L stainless steel and C52400 copper alloy

Yuchao Baia, Jiayi Zhanga, Cuiling Zhaoa, Chaojiang Lib, Hao Wanga,
a
Department of Mechanical Engineering, Faculty of Engineering, National University of Singapore, 9 Engineering Drive 1, Singapore 117575, Singapore
b
School of mechanical engineering, Beijing Institute of Technology, Zhongguancun Avenue, Haidian District, Beijing 100081, PR China

A R T I C LE I N FO A B S T R A C T

Keywords: Manufacturing multi-material part is one of the native advantages of selective laser melting (SLM) due to its
Selective laser melting layer-by-layer manufacturing method, which is attracting more and more attention in recent years. In an effort to
Multiple materials reveal the dual interfacial characterization of dissimilar materials manufactured by SLM with different printing
Microstructure sequences, this paper presents the morphology, microstructure, element distribution, phase composition and
316L stainless steel
microhardness of multi-material interfaces between SLMed 316L steel and C52400 copper alloy. Both interfaces
Copper alloy
Interfacial characterization
display isolated alloy islands with various shapes and different morphologies. The melt pool at 316L/C52400
interface is deeper and narrower than that at C52400/316L interface. Small 316L and C52400 spheres with a size
of 1–5 μm are formed under the surface tension, Marangoni convection in the melt pool and rapid cooling
condition, in which many smaller particles with a size of < 1 μm appear due to the material supersaturation and
convection. Interdiffusion of elements and very fine grains with a size of < 6 μm result in excellent metallurgical
bonding performance. Cracks tend to originate from the interface and extend to the stainless steel side for both
interfaces. No separation of the two materials caused by cracks is found in their contact area. Healing of the
cracks by C52400 copper alloy at 316L/C52400 interface is easier to complete. The interface thickness depends
on the building sequence of the two materials, which features a much thicker transition when building C52400
on 316L. No intermetallic compound but a trace of CuNi alloy is formed at the interface. The microhardness
varies in the transition area due to the existence of isolated 316L/C52400 islands and decreases from 316L to
C52400 with the highest value of 283.33 ± 5.51 HV to the lowest value of 181.33 ± 17.62 HV. This research
advances the understanding of the different interfacial characterizations of dissimilar materials manufactured by
SLM and provides guidance and reference for manufacturing multi-material components with complex interfaces
using SLM.

1. Introduction manufacturing single material, such as 316L steel, maraging steel,


aluminium alloy, CoCrW alloy, titanium alloy, copper alloy, etc.
Additive manufacturing (AM) technology provides a new method to [13–17] Besides, the process optimisation, microstructure, mechanical
manufacture various parts quickly, which has many advantages, in- properties, heat treatment and simulation have been reported by many
cluding high manufacturing freedom, excellent part performance and researchers [18–20].
high production efficiency [1–3]. Owing to its layer-by-layer manu- However, insufficient attention has been paid to manufacturing
facturing approach, AM is particularly suitable for manufacturing multilateral part using SLM. It is known that combining multiple ma-
multi-material parts, such as gradient materials, sandwich structure terials into one single part can enhance the properties and add value to
materials, etc. [4–8] As one of extensively applied AM technologies, final products. In the past, welding was used to combine dissimilar
selective laser melting (SLM) inherits the advantages of AM and is materials [21–24]. However, it is mainly applied in joining large pieces
especially capable of manufacturing metal parts using the laser beam to of dissimilar materials, which is difficult for fabricating small-size parts
melt metal powders [9,10]. Moreover, the SLM process has high cooling of an appreciable level of delicacy and impossible for changing material
rate (103–108 K/s), which improves the nucleation rate to refine grains in the designated position of the same part. SLM, however, can not only
for better properties [11,12]. Therefore, SLM is being widely used in programme the change of multiple materials but also accurately edit


Corresponding author.
E-mail address: mpewhao@nus.edu.sg (H. Wang).

https://doi.org/10.1016/j.matchar.2020.110489
Received 1 April 2020; Received in revised form 5 May 2020; Accepted 2 July 2020
Available online 07 July 2020
1044-5803/ © 2020 Elsevier Inc. All rights reserved.
Y. Bai, et al. Materials Characterization 167 (2020) 110489

the material composition within one layer thickness (~30 μm or less), SLMed parts was the zigzag scan mode with rotating 90° every two
which is more suitable for manufacturing multi-material part with the layers. Table 1 shows the chemical composition of 316L stainless steel
more uniform material distribution. One easy way using SLM to man- and C52400 copper alloy used in this study. 316L stainless steel part
ufacture multi-material part is to print one material on another material (10 × 10 × 3 mm) was built on a 316L stainless steel substrate at the
fabricated by a conventional manufacturing process such as casting room temperature, and then C52400 copper alloy part
[25,26]. Another way is to print one material on another SLMed ma- (10 × 10 × 3 mm) was built on the formerly manufactured 316L steel
terial [27,28]. The third way is to print different materials (such as substrate. Finally, a second 316L stainless steel layer
mixed powders) on the same layer [29]. Furthermore, SLM can also be (10 × 10 × 3 mm) was built on the as-printed layer of C52400 copper
used to print dissimilar materials, which are difficult to directly fuse via alloy. Fig. 1 displays the building process of dual interfacial materials
a metal interlayer such as copper alloy [30]. using SLM. For the change of different powders, it was manually done
For manufacturing multi-material parts using SLM, the key issue is by pausing the building process and changing for the other powders. To
the interfacial characterization between dissimilar materials, which reduce the negative effect of oxygen during powder changing, the air
determines the metallurgical bonding performance and corresponding was purged by argon from the printer chamber, and the building pro-
mechanical properties. Due to the melt pool characteristics of SLM, it is cess was not resumed until the oxygen level was below 200 ppm. Two
predicted that there will be multiple physical processes during manu- interfaces between 316L stainless steel and C52400 copper alloy were
facturing the interface: (1) Remelting of previous solid material; (2) formed. The interface between first 316L stainless steel part and
Mutual melting of multiple materials in the same melt pool; (3) C52400 copper alloy part is called 316L/C52400 interface, which is
Different solidification behaviours of the dissimilar materials in the referred to as the “L/C interface”. The interface between C52400 copper
same melt pool; and (4) The pinning effect on the previously built solid alloy and second 316L stainless steel part is called C52400/316L in-
layer with a curved melt pool. The abovementioned processes will take terface, which is referred to as the “C/L interface” in the context.
effects on the microstructure, grain morphology, element distribution,
mechanical properties, etc. Due to different material properties, the 2.2. Characterization
design of the printing sequence influences the interfacial characteriza-
tion, microstructure and mechanical properties. The state-of-the-art Microhardness was evaluated on the polished surface using Vickers
works on selective laser melted (SLMed) multi-material parts are fo- microhardness tester (SHIMADZU Corporation) with the load of 200 g
cused on printing one material on another SLMed material with dif- (1.961 N) and dwell time of 15 s according to ASTM E384-17. The
ferent printing order and corresponding solidification behaviour, mi- microhardness of each point was measured with three repetitions. X-ray
crostructure and element distribution at the interface as well as phase diffraction (XRD) patterns were achieved by a Bruker D8 Advanced
composition and microhardness. diffractometer system with Cu Kα radiation source after polishing the
Herein, this study aims to investigate the dual interfacial char- sample surface with #80, #400, #1000, #1500 and #2000 sandpapers.
acterization of 316L stainless steel-C52400 alloy parts manufactured by Electron backscattered diffraction (EBSD) was used to investigate the
SLM. Two interfaces combining dissimilar materials with different grain size and crystallographic orientation of the interfaces and ad-
printing orders are manufactured and investigated. The defects, such as jacent areas of the multi-material sample in Hitachi SU5000 SEM ma-
cracks, oxides and pores, formed at the interface are analysed. The chine with Hikari Super EBSD Camera. The microstructure was ob-
dynamic behaviour of melt pools at the interface during the SLM pro- served by a LEICA DM 2500 M metallographic microscope and JEOL
cess is characterised. The morphology, microstructure, element dis- JSM-5500LV scanning electron microscope (SEM) after polishing to a
tribution, phase composition and microhardness at the interfaces are mirror finish and etching using ferric chloride hydrochloric acid aqu-
investigated in details. The mechanism of multi-material interactions eous solution (FeCl: HCl: H2O = 3.5 g: 25 ml: 75 ml) for 2 s. The
during SLM is discussed. This study offers reference and guidance for chemical composition and element distribution on the interface were
the development and application of multi-material parts manufactured evaluated using energy-dispersive X-ray spectroscopy (EDS).
by SLM technology.

3. Results and discussion


2. Experiments
3.1. Microstructure and morphology
2.1. Sample preparation
The microstructure, morphology and chemical element distribution
All the experiments were carried out using a laser 3D printing ma- of SLMed C/L interface are shown in Fig. 2. From the optical micro-
chine SLS/SLM-3 V equipped with a 200 W IPG Yb fibre laser (wave- scope (OM) images after polishing (Fig. 2a), it can be seen that two
length: 1064 nm, laser beam diameter: 100 μm) and high-purity argon different colours present different metals: dark colour for 316L stainless
was used during the building process. The SLM parameters for 316L steel and orange colour for C52400 copper alloy. The mixing of metals
stainless steel were as follows: gas-atomised powder with a particle size at the interface is displayed clearly by embedding each other of two
distribution of 20–50 μm, laser power of 160 W, scanning speed of materials, which shows excellent metallurgical bonding characteristics
800 mm/s, hatching space of 0.09 mm, and layer thickness of 30 μm. without any cracks between C52400 material and 316L material. This
The SLM parameters for C52400 copper alloy were as follows: gas- result indicates that SLM can be used to manufacturing a multi-material
atomised powder with a particle size distribution of 15–45 μm, laser part using C52400 and 316L. At the C/L interface, 316L part becomes
power of 180 W, scanning speed of 300 mm/s, hatching space of interconnected and curved elongated blocks/bands, and many gaps are
0.08 mm and layer thickness of 30 μm. The scanning strategy for both formed between them and filled with copper alloy. Fig. 2b shows the

Table 1
Chemical composition (wt%) of 316L stainless steel and C52400 copper alloy.
Alloy name Cr Ni Mo C Mn P S Si N Fe

316L 16–18 10–14 2–3 ≤0.03 ≤2.0 ≤0.045 ≤0.03 ≤0.75 ≤0.1 Bal.
Alloy name Cu Sn Zn Pb Fe P
C52400 Bal. 9–11 ≤0.2 ≤0.05 ≤0.1 0.03–0.35

2
Y. Bai, et al. Materials Characterization 167 (2020) 110489

Fig. 1. Schematic diagram of additively manufactured dual interfaces of 316L stainless steel and C52400 copper alloy using SLM.

shallower and wider melt pools at the interface under SEM. Fig. 3 shows homogeneously due to the high cooling rate.
the microstructure, morphology and chemical element distribution of Beside the melt pool morphology, another difference between C/L
SLMed L/C interface, in which 316L and C52400 can also be dis- and L/C interfaces is seen that there is a significant transition at the L/C
tinguished with two different colours. interface marked by white dotted lines. However, no significant tran-
Comparing Figs. 2b and 3b, the melt pools at C/L interface are sition area can be found at the C/L interface. This transition is formed
shallower and wider comparing to the deeper and narrower melt pool at due to the C52400 melt pool flowing where the remelt 316L is mixed
the L/C interface. One reason is that the process parameters for printing with the copper alloy. Moreover, the contents of 316L and C52400 are
316L steel are different from that printing C52400 copper alloy, which similar, which can be seen in the EDS mapping images of both inter-
have different energy density. Another important reason is that the heat faces between 316L and C52400 as shown in Figs. 2d, e, 3d, e. Besides,
conductivity of 316L (16.2 W/m·K) is lower than C52400 copper alloy the distribution of Fe and Cu elements further displays the boundaries
(50 W/m·K). More heat can be absorbed to melt the pre-built 316L part. between two different SLMed metals at the interfaces and the inter-
Moreover, isolated 316L blocks (marked by blue arrows) with irregular diffusion of elements.
size and shape appear in the area far from the interface and near the High magnification images of both interfaces were obtained using
copper side in Fig. 2a, and isolated copper blocks (marked by blue ar- SEM after etching as shown in Figs. 4 and 5. Both interfaces are re-
rows) are also embedded in the pre-built 316L part in Fig. 3a. One vealed between 316L and C52400 parts, in which very small particles
reason is that high undercooling leads to liquid phase separation (< 1 μm in size) are formed as shown in Figs. 4B and 5E. EDS mapping
[31–34]. Another reason is the disturbance of the melt pool under the results (Figs. 2 and 3) show that these regions are the mixtures of 316L
effect of the laser beam as well as the complex and non-uniform metal and C52400 because substantial Fe and Cu elements are found to co-
liquid flowing [35], which transfers the material from one place to exist. According to Fig. 5E and the chemical composition in Table 2,
another place [30,36]. Solidification occurs before they can mingle approximately spherical particles are mainly composed of 316L and the

Fig. 2. Microstructure, morphology and chemical element distribution at C/L interface: (a) Optical image; (b) SEM image; (c) (d) (e) Fe and Cu element distribution
at the interface using EDS mapping.

3
Y. Bai, et al. Materials Characterization 167 (2020) 110489

Fig. 3. Microstructure, morphology and chemical element distribution at L/C interface: (a) Optical image; (b) SEM image; (c) (d) (e) Fe and Cu element distributions
at the interface using EDS mapping.

irregular particles are mainly composed of C52400. This is because Fe microstructure near 316L sides, in which the melt pools can be seen and
and Cu are infinitely soluble in the liquid state and limitedly soluble in some copper blocks are embedded in the 316L part. However, near the
the solid state. Due to the higher melt point, 316L will solidify first and C52400 sides, Fig. 4C presents the sawtooth shape without well-defined
tend to form spheres to reduce surface free energy. Then, liquid-state melt pools. Fig. 5D shows the feathery morphology which features the
C52400 fulfils the gaps between the pre-solidified 316L particles and microstructure of SLMed copper alloy [37].
solidified into irregular shapes. Figs. 4A and 5F display the

Fig. 4. High magnification microstructure at the C/L interface after etching.

4
Y. Bai, et al. Materials Characterization 167 (2020) 110489

Fig. 5. High magnification microstructure at the L/C interface after etching.

Table 2 to the higher thermal conductivity of C52400 than 316L, the absorbed
Chemical composition (wt%) results from the microstructure as shown in energy by 316L melt pool is much lower than that when building 316L
Fig. 5E. on the 316L substrate material. This condition is equivalent to the
Element Fe Cr Ni Mo Si Cu Sn condition for manufacturing 316L with low laser power or low energy
density, which results in the formation of various defects such as large
Spectrum 1 36.63 9.77 7.48 1.56 0.92 39.18 4.45 cracks, holes, or pores [41,42].
Spectrum 2 7.76 2.57 5.19 – – 74.5 9.98
Cracks filled with copper alloy were also found in Fig. 3a (marked
by the yellow arrow), which means that some of the crack defects can
be eliminated and the metallurgical bond between crack interface and
3.2. Defects
copper alloy can be improved to mitigate the negative effect on the
mechanical properties [43]. However, large cracks are formed near the
Cracks (marked by the yellow arrows) can be observed at the in-
316L sides (shown by yellow arrows in Figs. 2c and 3c, and green da-
terface near 316L side in Fig. 2c, and in the pre-built 316L part near the
shed box in Fig. 5F) which are not filled or partially filled with copper
melt pool as shown in Fig. 3a and c. This is mainly caused by the dif-
alloy. For the L/C interface, the massive cracks cannot be filled com-
ference in physical properties between 316L and C52400 such as
pletely by the copper alloy before solidification because of the large size
thermal expansion, heat conduction and melt points, resulting in the
of these cracks. For the C/L interface, one reason is that the density of
stress mismatch [28,38]. Similar phenomena can be seen during
C52400 is higher than that of 316L which leads to less C52400 material
welding of copper and iron base material, in which a small amount of
near the 316L side. Another reason is the lower melt point of 316L
copper penetrates the border of 316L stainless steel and a brittle copper
which will solidify first and the crack is far from the interface, such that
film with low strength is formed. In the subsequent cooling process, due
the melted copper is blocked by the solidified 316L part from entering
to the differences in the thermophysical properties between copper and
the cracks. Similar phenomena can also be observed in the completely
stainless steel, the degree of shrinkage between copper and steel is not
and partially filled cracks with copper in electrical beam freeform
consistent, which results in high residual stress and thermal penetration
fabrication of copper/steel thin-wall parts [44]. Other types of defects
cracks in the steel side [39,40]. The cracks originate from the interface
are also evident, such as black spots marked by the white arrow in
and extend to the 316L side (as shown by yellow arrows in Figs. 4 and
Fig. 3a and pores marked by black arrows in Fig. 5. The black spots are
5), which also substantiates the above analysis. Fig. 6 displays the crack
mainly caused by oxidation. The oxides appear in the melt pool because
distribution at the C/L and L/C interfaces, respectively. It can be seen
they are too heavy to be brought to the interface of the melt pool by the
that there are few cracks in the transition area and near the copper side,
Marangoni convection [45]. Cracks, oxides and pores are undesirable
which indicates that high content of copper and low content of 316L
for the properties of SLMed multi-material parts. They should be
will not lead to cracks during SLM process. Some big cracks (marked by
eliminated by designing better process parameters and reducing the
the yellow dashed circle) with different directions are shown near 316L
oxygen content in the building process.
side at the C/L interface in Fig. 6a. These cracks are caused not only by
thermal penetration crack but also by the process parameter mismatch.
During the whole SLM process, the process parameters for 316L remain
the same. However, when building 316L on the pre-built C52400, due

5
Y. Bai, et al. Materials Characterization 167 (2020) 110489

Fig. 6. Cracks distribution at (a) the C/L interface and (b) the L/C interface.

Fig. 7. SEM and EBSD images at the SLMed C/L interface: (a) Testing region; (b) EBSD result; (c)(d)(e) Pole figures and (I): Microstructure after polishing corre-
sponding to (b).

3.3. Texture characterization (001), (101) and (111). A few large grains in the fine grain region are
316L blocks which move to the transition area due to the liquid metal
Phase detection results at the C/L interface using EBSD show that flow. Moreover, obtained from the pole figure, Brass {011}⟨211⟩ and
only a face-centre cubic (FCC) structure is found in the whole interface, Copper{112}⟨111⟩ are the main orientations in Region c, Cube{110}
which are γ-Fe and ε-Cu phases [46], as shown in Fig. 7b. The ⟨001⟩ and Brass are the main orientations in the transition Region d,
boundaries between 316L part, transition area and C52400 part can be and Goss {011}⟨100⟩ and Cube mainly exist in Region e.
seen clearly. The fine grains in the grain size measurements obtained EBSD was also performed on the L/C interface as shown in Fig. 8.
from EBSD characterization at the C/L interface displayed that the in- Fine grains are also found in the transition area. However, the width of
terface region has the smallest size with an average value of 5.66 μm, the L/C transition (~550 μm) is much larger than that of the C/L
compared with the C52400 regions of 8.29 μm and 316L of 13.53 μm, transition (~170 μm). Besides the liquid melt pool flowing caused by
as shown in Figs. 9a, b and c. The main reason for the formation of fine Marangoni convection, another reason is the lower density of 316L than
grain is that the pre-solidified 316L particles offer the cores for the C52400. Therefore, more 316L liquid can float up in the liquid melt
subsequent grain growth. Another reason for fine grains is the melt pool pool. Besides, compared with the pre-built copper alloy part, the lower
flowing and Rayleigh-Taylor instability which result in the local tur- heat conductivity of pre-built 316L reduces the heat loss, increases melt
bulence occurring in the contact area between C52400 liquid droplet pool volume and is conducive to melting more material, which offers
and 316L liquid droplet. Therefore, much smaller droplets are formed. the more time for 316L liquid to float up to the upper. When the next
The third reason is secondary phase separation from the highly super- laser scans the powders, the 316L in the upper of the previous layer will
saturated Fe-rich matrix and Cu-rich matrix during solidification. Ul- continue to float up following the liquid metal in the melt pool. How-
trafine grain was also found during additive manufacturing titanium ever, the size of fine grain (5.16 μm) only has negligible change com-
alloy by blending pure titanium powders and copper powders [47]. pared with the C/L interface (5.66 μm), as well as the grain size of the
Regions c, d and e present significant orientated anisotropy, along 316L part and C52400 part, as shown in Fig. 9c, d and e. Similarly,

6
Y. Bai, et al. Materials Characterization 167 (2020) 110489

Fig. 8. SEM and EBSD images at the SLMed L/C interface: (a) Testing region; (b) EBSD; (c) (d) (e) Pole figures and (II) Microstructure after polishing corresponding to
(b).

some big 316L blocks are found in the transition area near the 316L 3.4. Material distribution behaviour
side. In Fig. 8d, the orientations show more dispersion compared with
Region d in Fig. 7b. From the pole figure, Cube is the main orientation Fig. 10a and b display the typical two-phase microstructure in
in Region c, Goss and Copper are main orientations existing in transi- CueFe base alloys [48], in which small Fe-rich particles are formed in
tion Region d, and Brass and Copper are the main orientations in Region large Cu matrix sphere, as well as small Cu-rich particles in large Fe
e. Compared with the orientations in Fig. 7, the orientations of the matrix sphere. The large spheres are mainly due to the liquid metal
transition zone show significant variations in texture components. As flowing, i.e. liquid metal (316L or C52400) transporting from one lo-
for the 316L and C52400 parts, the same main texture components are cation to another. It is because the thermal distribution in the melt pool
maintained as orientations in Fig. 7. is uneven when the laser melts the powders and remelts the pre-built
part [49,50]. Therefore, a large surface tension gradient is formed as
well as resultant Marangoni convection, which takes effects on the

Fig. 9. Grain size distribution at the dual interfacial regions: (a) (b) (c) at the L/C interface; (d) (e) (f) at the C/L interface.

7
Y. Bai, et al. Materials Characterization 167 (2020) 110489

Fig. 10. (a) Melt behaviour at the L/C interface; (b) Melt pool behaviour at the C/L interface.

Fig. 11. Diagram of melted material behaviour during SLM: (a) C/L interface; (b) L/C interface.

melting dynamics, mass and heat transfer [51–53]. Fig. 11 shows the (marked by white arrows). One reason is that the vapour generated
mass transfer of melted material during SLM of dissimilar materials. It during SLM did not escape from the melt pool in time, resulting in the
can be known that C52400 is brought to 316L side at the C/L interface formation of holes. Another important reason is that the shrinkage due
and 316L is brought to C52400 side at the L/C interface, which results to solidification of the liquid copper alloy with a reduction in volume
in the mixture of both materials. However, due to the difference in and the pre-solidified stainless steel in the surroundings hinder the re-
surface tension between FeeFe and CueCu and high cooling rate, the plenishment of the copper alloy liquid. Chen et al. [44] also found si-
same material tends to aggregate instead of being scattered to blocks. milar holes due to the shrinkage of copper alloy when studying the
Also, the rising metal vapour lifts up part of the material at the bottom. copper/304 steel gradient composite materials fabricated by electron
Some smaller particles are found inside the large ones due to the effect beam freeform process.
of liquid metal flow that transfers and breaks the material into small The EDS results corresponding to Fig. 10a and b are shown in
droplets. This phenomenon comes mainly from the supersaturated solid Table 3. Both 316L matrix and C52400 matrix are highly super-
solution formed during SLM process due to rapid solidification, which is saturated because of high contents of other elements. Fig. 12a and b
called secondary phase separation [54,55]. It can be seen that some display the distribution of chemical elements across the interfaces using
holes are formed at both interfaces, especially in the Cu-rich blocks EDS line scan, which gives a clear composition change. Similar step

8
Y. Bai, et al. Materials Characterization 167 (2020) 110489

Table 3
Main chemical composition (wt%) measured from the microstructure of Fig. 9.
Element P1 P2 P3 P4 P5 P6 P7 P8 P9 P10 P11 P12

Fe 36.22 13.11 45.45 11.97 56.08 11.23 22.13 52.65 17.56 44.60 11.05 46.12
Cr 10.53 3.62 12.69 3.73 15.15 3.00 6.39 14.87 5.13 12.14 5.29 13.46
Ni 7.82 5.41 8.12 4.38 6.97 3.37 5.14 7.23 4.62 9.83 5.06 8.86
Cu 39.15 70.29 24.35 72.40 14.25 71.80 59.44 17.22 62.89 25.31 64.25 24.02
Sn 5.43 7.03 3.44 7.52 1.02 10.59 6.89 2.15 9.80 4.82 13.66 3.31

change and larger transition region appear at the L/C interface. The 4. Conclusions
drastic fluctuations of the profiles are caused by the isolated 316L and/
or C52400 blocks distributed at the interface due to the limited mis- In this work, dual interfaces between 316L stainless steel and
cibility between 316L and C52400 during SLM. C52400 copper alloy are manufactured successfully by SLM, and dif-
ferent characterizations between two interfaces are presented. The
microstructure, interface morphology, defects, elemental composition,
3.5. Phase composition and microhardness phase composition and microhardness are characterised. The primary
findings of this study are as follows:
Fig. 13a shows the XRD patterns of L/C interface, including the steel
side, copper side and transition region. It is clear to see that the XRD • Different isolated alloy islands are found at both interfaces. At the
pattern of the transition region combines the 316L steel and C52400 C/L interface, 316L part becomes interconnected and curved elon-
copper alloy. Besides, broadening and shifting of diffraction peaks ap- gated blocks/bands, and many gaps are formed between them and
pear at the transition area, which is mainly caused by the fine grains filled with copper alloy. At the L/C interface, some copper blocks are
and residual stress formed during SLM [56,57]. According to the XRD formed in the pre-built 316L part, and the melt pool is much deeper
patterns and phase diagram of FeeCu, none Fe/Cu intermetallic com- and narrower. After etching, serrated morphology is found near
pounds are formed in the transition area [48]. A small peak (marked by C52400 side at the C/L interface compared with the feathered mi-
black arrow) appears in the transition area, which is likely the CuNi crostructure at the L/C interface.
alloy [58–60]. • Small 316L and C52400 spheres with a size of 1–5 μm are formed
The microhardness was measured across the interfacial regions of under the surface tension and Marangoni convection in the melt
both L/C and C/L to investigate the evolution laws of microhardness pool due to the rapid cooling. Smaller particles with a size of below
along the building direction as shown in Fig. 13b. The microhardness of 1 μm are formed in these spheres due to the precipitation of su-
the above two interfaces was measured from the steel side to the copper persaturated solid solution besides the effect of convection.
side and then steel side with a total of 24 points. The average micro- • Excellent metallurgical bonding performance between the two me-
hardness of the L/C interface decreases from 283.33 ± 5.51 HV to tals is obtained by mixing metals at the interfaces with no separation
181.33 ± 17.62 HV, compared with the C/L interface increasing from between the contact area between 316L and C52400. 316L/C52400
188.00 ± 2.65 HV to 268.00 ± 7.00 HV. At the C/L interface, the interface displays a better combination with fewer cracks, some of
microhardness value fluctuates greatly compared with the L/C interface which are filled with cooper alloy, as well as wider transition re-
area. This is because the large isolated 316L blocks distribute at the gions due to the lower heat conductivity and density of pre-built
interface, which has higher microhardness than the interfacial area. The 316L part. Both interfaces display fine grains with an average size of
chemical element distributions at both interfaces are illustrated in 5–6 μm in the transition zone, compared with the single metal re-
Fig. 11. The microhardness near the copper side at C/L interface is a gions with average grain sizes above 13 μm for 316L and 8 μm for
slightly larger than that at the L/C interface, which may be caused by C52400.
the finer grains, as shown in Figs. 7–9. • Cracks extending to the 316L side, oxides and pores in the melt pool
are the main defects at the interface. The cracks are mainly caused
by parameter mismatch and stress mismatch because of different

Fig. 12. (a) EDS line scan at the C/L interface; (b) EDS line scan at the L/C interface.

9
Y. Bai, et al. Materials Characterization 167 (2020) 110489

Fig. 13. (a) XRD patterns of single metal and transition; (b) Microhardness along the building direction.

thermal expansion, heat conduction and melt points between 316L steel and inconel 625 fabricated by directed energy deposition: characterization and
and C52400. thermodynamic modeling, Acta Mater. 108 (2016) 46–54, https://doi.org/10.


1016/j.actamat.2016.02.019.
XRD patterns indicate that no obvious intermetallic compounds are [9] Y. Bai, Y. Yang, D. Wang, M. Zhang, Influence mechanism of parameters process
produced during manufacturing but a trace of CuNi alloy. The mi- and mechanical properties evolution mechanism of maraging steel 300 by selective
crohardness decreases gradually from the 316L side to C52400 side laser melting, Mater. Sci. Eng. A 703 (2017) 116–123, https://doi.org/10.1016/j.
msea.2017.06.033.
with 283.33 ± 5.51 HV to 181.33 ± 17.62 HV at L/C interface [10] B. Chen, S.K. Moon, X. Yao, G. Bi, J. Shen, J. Umeda, K. Kondoh, Strength and strain
and 268.00 ± 7.00 HV to 188.00 ± 2.65 HV at C/L interface, hardening of a selective laser melted AlSi10Mg alloy, Scr. Mater. 141 (2017) 45–49,
respectively. https://doi.org/10.1016/j.scriptamat.2017.07.025.
[11] T. Vilaro, V. Kottman-Rexerodt, M. Thomas, C. Colin, P. Bertrand, L. Thivillon,
S. Abed, V. Ji, P. Aubry, P. Peyre, T. Malot, Direct fabrication of a Ti-47Al-2Cr-2Nb
Declaration of competing interest alloy by selective laser melting and direct metal deposition processes, Adv. Mater.
Res. 89–91 (2010) 586–591, https://doi.org/10.4028/www.scientific.net/AMR.89-
91.586.
The authors declare that they have no known competing financial [12] X.P. Li, X.J. Wang, M. Saunders, A. Suvorova, L.C. Zhang, Y.J. Liu, M.H. Fang,
interests or personal relationships that could have appeared to influ- Z.H. Huang, T.B. Sercombe, A selective laser melting and solution heat treatment
ence the work reported in this paper. refined Al-12Si alloy with a controllable ultrafine eutectic microstructure and 25%
tensile ductility, Acta Mater. 95 (2015) 74–82, https://doi.org/10.1016/j.actamat.
2015.05.017.
Acknowledgements [13] D. Wang, C. Song, Y. Yang, Y. Bai, Investigation of crystal growth mechanism
during selective laser melting and mechanical property characterization of 316L
stainless steel parts, Mater. Des. 100 (2016) 291–299, https://doi.org/10.1016/j.
This work is supported by the Ministry of Education - Singapore matdes.2016.03.111.
AcRF Tier 1 (Project No.: R-265-000-686-114). [14] Y. Bai, Y. Yang, Z. Xiao, M. Zhang, D. Wang, Process optimization and mechanical
property evolution of AlSiMg0.75 by selective laser melting, Mater. Des. 140 (2018)
257–266, https://doi.org/10.1016/j.matdes.2017.11.045.
Data availability [15] Y. Bai, D. Wang, Y. Yang, H. Wang, Effect of heat treatment on the microstructure
and mechanical properties of maraging steel by selective laser melting, Mater. Sci.
The raw/processed data required to reproduce these findings cannot Eng. A 760 (2019) 105–117, https://doi.org/10.1016/j.msea.2019.05.115.
[16] Y. Bai, Z. Shi, Y.J. Lee, H. Wang, Optical surface generation on additively manu-
be shared at this time as the data also forms part of an ongoing study. factured AlSiMg0.75 alloys with ultrasonic vibration-assisted machining, J. Mater.
Process. Technol. 280 (2020) 116597. doi:https://doi.org/10.1016/j.jmatprotec.
References 2020.116597.
[17] D. Wang, G. Ye, W. Dou, M. Zhang, Y. Yang, S. Mai, Y. Liu, Influence of spatter
particles contamination on densification behavior and tensile properties of CoCrW
[1] I. Gibson, D. Rosen, B. Stucker, Additive Manufacturing Technologies, Springer New manufactured by selective laser melting, Opt. Laser Technol. 121 (2020) 105678,
York, New York, NY, 2014, https://doi.org/10.1007/978-1-4939-2113-3. https://doi.org/10.1016/j.optlastec.2019.105678.
[2] K.K. Parker, Additive manufacturing of metals, Acta Mater. 117 (2016) 371–392, [18] C. Panwisawas, C.L. Qiu, Y. Sovani, J.W. Brooks, M.M. Attallah, H.C. Basoalto, On
https://doi.org/10.1016/j.actamat.2016.07.019. the role of thermal fluid dynamics into the evolution of porosity during selective
[3] Y. Bai, A. Chaudhari, H. Wang, Investigation on the microstructure and machin- laser melting, Scr. Mater. 105 (2015) 14–17, https://doi.org/10.1016/j.scriptamat.
ability of ASTM A131 steel manufactured by directed energy deposition, J. Mater. 2015.04.016.
Process. Technol. 276 (2020) 116410, https://doi.org/10.1016/j.jmatprotec.2019. [19] J. Wu, X.Q. Wang, W. Wang, M.M. Attallah, M.H. Loretto, Microstructure and
116410. strength of selectively laser melted AlSi10Mg, Acta Mater. 117 (2016) 311–320,
[4] L.D. Bobbio, R.A. Otis, J.P. Borgonia, R.P. Dillon, A.A. Shapiro, Z.K. Liu, A.M. Beese, https://doi.org/10.1016/j.actamat.2016.07.012.
Additive manufacturing of a functionally graded material from Ti-6Al-4V to invar: [20] S.M.H. Hojjatzadeh, N.D. Parab, W. Yan, Q. Guo, L. Xiong, C. Zhao, M. Qu,
experimental characterization and thermodynamic calculations, Acta Mater. 127 L.I. Escano, X. Xiao, K. Fezzaa, W. Everhart, T. Sun, L. Chen, Pore elimination
(2017) 133–142, https://doi.org/10.1016/j.actamat.2016.12.070. mechanisms during 3D printing of metals, Nat. Commun. 10 (2019) 1–8, https://
[5] J.S. Zuback, T.A. Palmer, T. DebRoy, Additive manufacturing of functionally graded doi.org/10.1038/s41467-019-10973-9.
transition joints between ferritic and austenitic alloys, J. Alloys Compd. 770 (2019) [21] K.J. Lee, S. Kumai, Characterization of intermetallic compound layer formed at the
995–1003, https://doi.org/10.1016/j.jallcom.2018.08.197. weld interface of the defocused laser welded low carbon steel/6111 aluminum alloy
[6] A. Bandyopadhyay, B. Heer, Additive manufacturing of multi-material structures, lap joint, Mater. Trans. 47 (2006) 1178–1185, https://doi.org/10.2320/matertrans.
Mater. Sci. Eng. R. Rep. 129 (2018) 1–16, https://doi.org/10.1016/j.mser.2018.04. 47.1178.
001. [22] Y. Shi, H. Zhang, T. Watanabe, J. Tang, CW/PW dual-beam YAG laser welding of
[7] G.H. Loh, E. Pei, D. Harrison, M.D. Monzón, An overview of functionally graded steel/aluminum alloy sheets, Zhongguo Jiguang/Chinese J. Lasers. 37 (2010)
additive manufacturing, Addit. Manuf. 23 (2018) 34–44, https://doi.org/10.1016/ 1132–1137, https://doi.org/10.3788/CJL20103704.1132.
j.addma.2018.06.023. [23] M.J. Torkamany, S. Tahamtan, J. Sabbaghzadeh, Dissimilar welding of carbon steel
[8] B.E. Carroll, R.A. Otis, J.P. Borgonia, J.O. Suh, R.P. Dillon, A.A. Shapiro, to 5754 aluminum alloy by Nd:YAG pulsed laser, Mater. Des. 31 (2010) 458–465,
D.C. Hofmann, Z.K. Liu, A.M. Beese, Functionally graded material of 304L stainless https://doi.org/10.1016/j.matdes.2009.05.046.

10
Y. Bai, et al. Materials Characterization 167 (2020) 110489

[24] S. Chen, L. Li, Y. Chen, J. Dai, J. Huang, Improving interfacial reaction non- 112 (2016) 328–338, https://doi.org/10.1016/j.matdes.2016.09.043.
homogeneity during laser welding-brazing aluminum to titanium, Mater. Des. 32 [43] U. Articek, M. Milfelner, I. Anzel, Synthesis of functionally graded material H13/Cu
(2011) 4408–4416, https://doi.org/10.1016/j.matdes.2011.03.074. by LENS technology, Adv. Prod. Eng. Manag. 8 (2013) 169–176. doi:10.14743/
[25] S. Shakerin, A. Hadadzadeh, B.S. Amirkhiz, S. Shamsdini, J. Li, M. Mohammadi, apem2013.3.164.
Additive manufacturing of maraging steel-H13 bimetals using laser powder bed [44] G. Chen, X. Shu, J. Liu, B. Zhang, J. Feng, Crystallographic texture and mechanical
fusion technique, Addit. Manuf. 29 (2019) 100797, https://doi.org/10.1016/j. properties by electron beam freeform fabrication of copper/steel gradient compo-
addma.2019.100797. site materials, Vacuum. 171 (2020) 109009, https://doi.org/10.1016/j.vacuum.
[26] C. Tan, K. Zhou, W. Ma, L. Min, Interfacial characteristic and mechanical perfor- 2019.109009.
mance of maraging steel-copper functional bimetal produced by selective laser [45] T.N. Le, Y.L. Lo, Effects of sulfur concentration and Marangoni convection on melt-
melting based hybrid manufacture, Mater. Des. 155 (2018) 77–85, https://doi.org/ pool formation in transition mode of selective laser melting process, Mater. Des.
10.1016/j.matdes.2018.05.064. 179 (2019) 107866, https://doi.org/10.1016/j.matdes.2019.107866.
[27] S.L. Sing, L.P. Lam, D.Q. Zhang, Z.H. Liu, C.K. Chua, Interfacial characterization of [46] Y.Z. Chen, F. Liu, G.C. Yang, X.Q. Xu, Y.H. Zhou, Rapid solidification of bulk un-
SLM parts in multi-material processing: intermetallic phase formation between dercooled hypoperitectic Fe-Cu alloy, J. Alloys Compd. 427 (2007) 3–8, https://doi.
AlSi10Mg and C18400 copper alloy, Mater. Charact. 107 (2015) 220–227, https:// org/10.1016/j.jallcom.2006.03.012.
doi.org/10.1016/j.matchar.2015.07.007. [47] D. Zhang, D. Qiu, M.A. Gibson, Y. Zheng, H.L. Fraser, D.H. StJohn, M.A. Easton,
[28] J. Chen, Y. Yang, C. Song, M. Zhang, S. Wu, D. Wang, Interfacial microstructure and Additive manufacturing of ultrafine-grained high-strength titanium alloys, Nature.
mechanical properties of 316L /CuSn10 multi-material bimetallic structure fabri- 576 (2019) 91–95, https://doi.org/10.1038/s41586-019-1783-1.
cated by selective laser melting, Mater. Sci. Eng. A 752 (2019) 75–85, https://doi. [48] R.P. Shi, C.P. Wang, D. Wheeler, X.J. Liu, Y. Wang, Formation mechanisms of self-
org/10.1016/j.msea.2019.02.097. organized core/shell and core/shell/corona microstructures in liquid droplets of
[29] C. Wei, L. Li, X. Zhang, Y.H. Chueh, 3D printing of multiple metallic materials via immiscible alloys, Acta Mater. 61 (2013) 1229–1243, https://doi.org/10.1016/j.
modified selective laser melting, CIRP Ann. 67 (2018) 245–248, https://doi.org/10. actamat.2012.10.033.
1016/j.cirp.2018.04.096. [49] D. Gu, H. Wang, D. Dai, P. Yuan, W. Meiners, R. Poprawe, Rapid fabrication of Al-
[30] C.F. Tey, X. Tan, S.L. Sing, W.Y. Yeong, Additive manufacturing of multiple ma- based bulk-form nanocomposites with novel reinforcement and enhanced perfor-
terials by selective laser melting: Ti-alloy to stainless steel via a cu-alloy interlayer, mance by selective laser melting, Scr. Mater. 96 (2015) 25–28, https://doi.org/10.
Addit. Manuf. 31 (2019) 100970, https://doi.org/10.1016/J.ADDMA.2019. 1016/j.scriptamat.2014.10.011.
100970. [50] D. Gu, Y.C. Hagedorn, W. Meiners, G. Meng, R.J.S. Batista, K. Wissenbach,
[31] S. Chen, J. Huang, J. Xia, X. Zhao, S. Lin, Influence of processing parameters on the R. Poprawe, Densification behavior, microstructure evolution, and wear perfor-
characteristics of stainless steel/copper laser welding, J. Mater. Process. Technol. mance of selective laser melting processed commercially pure titanium, Acta Mater.
222 (2015) 43–51, https://doi.org/10.1016/j.jmatprotec.2015.03.003. 60 (2012) 3849–3860, https://doi.org/10.1016/j.actamat.2012.04.006.
[32] S. Chen, J. Huang, J. Xia, H. Zhang, X. Zhao, Microstructural characteristics of a [51] C.L.A. Leung, S. Marussi, R.C. Atwood, M. Towrie, P.J. Withers, P.D. Lee, In situ X-
stainless steel/copper dissimilar joint made by laser welding, Metall. Mater. Trans. ray imaging of defect and molten pool dynamics in laser additive manufacturing,
A Phys. Metall. Mater. Sci. 44 (2013) 3690–3696, https://doi.org/10.1007/s11661- Nat. Commun. 9 (2018) 1–9, https://doi.org/10.1038/s41467-018-03734-7.
013-1693-z. [52] S.A. Khairallah, A.T. Anderson, A.M. Rubenchik, W.E. King, Laser powder-bed fu-
[33] R.M. Miranda, E. Assunção, R.J.C. Silva, J.P. Oliveira, L. Quintino, Fiber laser sion additive manufacturing: physics of complex melt flow and formation me-
welding of NiTi to Ti-6Al-4V, Int. J. Adv. Manuf. Technol. 81 (2015) 1533–1538, chanisms of pores, spatter, and denudation zones, Addit. Manuf. Handb. Prod. Dev.
https://doi.org/10.1007/s00170-015-7307-8. Def. Ind. 108 (2017) 613–628, https://doi.org/10.1201/9781315119106.
[34] J. Li, Y. Liu, Z. Zhen, P. Jin, Q. Sun, J. Feng, Weld formation mechanism and mi- [53] C. Zhao, K. Fezzaa, R.W. Cunningham, H. Wen, F. De Carlo, L. Chen, A.D. Rollett,
crostructural evolution of TC4/304 stainless steel joint with Cu-based filler wire and T. Sun, Real-time monitoring of laser powder bed fusion process using high-speed X-
preheating, Materials (Basel) 12 (2019) 3071, https://doi.org/10.3390/ ray imaging and diffraction, Sci. Rep. 7 (2017) 1–11, https://doi.org/10.1038/
ma12193071. s41598-017-03761-2.
[35] R.P. Shi, Y. Wang, C.P. Wang, X.J. Liu, Self-organization of core-shell and core- [54] G. Salje, M. Feller-Kniepmeier, The diffusion and solubility of iron in copper, J.
shell-corona structures in small liquid droplets, Appl. Phys. Lett. 98 (2011) Appl. Phys. 49 (1978) 229–232, https://doi.org/10.1063/1.324336.
2009–2012, https://doi.org/10.1063/1.3591157. [55] T. Toyama, F. Takahama, A. Kuramoto, H. Takamizawa, Y. Nozawa, N. Ebisawa,
[36] S.A. David, J.M. Vitek, Correlation between solidification parameters and weld M. Shimodaira, Y. Shimizu, K. Inoue, Y. Nagai, The diffusivity and solubility of
microstructures, Int. Mater. Rev. 34 (1989) 213–245, https://doi.org/10.1179/imr. copper in ferromagnetic iron at lower temperatures studied by atom probe tomo-
1989.34.1.213. graphy, Scr. Mater. 83 (2014) 5–8, https://doi.org/10.1016/j.scriptamat.2014.03.
[37] Z.H. Liu, D.Q. Zhang, S.L. Sing, C.K. Chua, L.E. Loh, Interfacial characterization of 009.
SLM parts in multi-material processing: metallurgical diffusion between 316L [56] Y. Kok, X. Tan, S.B. Tor, C.K. Chua, Fabrication and microstructural characterisa-
stainless steel and C18400 copper alloy, Mater. Charact. 94 (2014) 116–125, tion of additive manufactured Ti-6Al-4V parts by electron beam melting: this paper
https://doi.org/10.1016/j.matchar.2014.05.001. reports that the microstructure and micro-hardness of an EMB part is thickness
[38] B. Talic, P.V. Hendriksen, K. Wiik, H.L. Lein, Thermal expansion and electrical dependent, Virtual Phys. Prototyp. 10 (2015) 13–21, https://doi.org/10.1080/
conductivity of Fe and Cu doped MnCo2O4 spinel, Solid State Ionics 326 (2018) 17452759.2015.1008643.
90–99, https://doi.org/10.1016/j.ssi.2018.09.018. [57] Z. Sun, X. Tan, S.B. Tor, W.Y. Yeong, Selective laser melting of stainless steel 316L
[39] Z. Cheng, J. Huang, Z. Ye, Y. Chen, J. Yang, S. Chen, Microstructures and me- with low porosity and high build rates, Mater. Des. 104 (2016) 197–204, https://
chanical properties of copper-stainless steel butt-welded joints by MIG-TIG double- doi.org/10.1016/j.matdes.2016.05.035.
sided arc welding, J. Mater. Process. Technol. 265 (2019) 87–98, https://doi.org/ [58] W. Yi, J. Liu, H. Chen, Y. Gao, H. Li, Copper/nickel nanoparticle decorated carbon
10.1016/j.jmatprotec.2018.10.007. nanotubes for nonenzymatic glucose biosensor, J. Solid State Electrochem. 19
[40] J. Kar, S.K. Roy, G.G. Roy, Effect of beam oscillation on electron beam welding of (2015) 1511–1521, https://doi.org/10.1007/s10008-015-2766-2.
copper with AISI-304 stainless steel, J. Mater. Process. Technol. 233 (2016) [59] A. Ungureanu, B. Dragoi, A. Chirieac, S. Royer, D. Duprez, E. Dumitriu, Synthesis of
174–185, https://doi.org/10.1016/j.jmatprotec.2016.03.001. highly thermostable copper-nickel nanoparticles confined in the channels of or-
[41] J.A. Cherry, H.M. Davies, S. Mehmood, N.P. Lavery, S.G.R. Brown, J. Sienz, dered mesoporous SBA-15 silica, J. Mater. Chem. 21 (2011) 12529–12541, https://
Investigation into the effect of process parameters on microstructural and physical doi.org/10.1039/c1jm10971e.
properties of 316L stainless steel parts by selective laser melting, Int. J. Adv. Manuf. [60] J. Yang, X. Shen, Z. Ji, H. Zhou, G. Zhu, K. Chen, In situ growth of hollow CuNi alloy
Technol. 76 (2014) 869–879, https://doi.org/10.1007/s00170-014-6297-2. nanoparticles on reduced graphene oxide nanosheets and their magnetic and cat-
[42] A. Ahmadi, R. Mirzaeifar, N.S. Moghaddam, A.S. Turabi, H.E. Karaca, M. Elahinia, alytic properties, Appl. Surf. Sci. 316 (2014) 575–581, https://doi.org/10.1016/j.
Effect of manufacturing parameters on mechanical properties of 316L stainless steel apsusc.2014.08.097.
parts fabricated by selective laser melting: a computational framework, Mater. Des.

11

You might also like