Materials Letters 267 (2020) 127547

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

Effect of microwave treatment on bending properties of carbon

nanotube/wood plastic composites by selective laser sintering
Yunhe Zhang a,⇑, Yanhong Cui a, Sian Wang a, Xiwang Zhao a, Fanming Wang a, Gaohui Wu b
a
College of Mechanical and Electrical Engineering, Northeast Forestry University, Harbin, PR China
b
School of Materials Science and Engineering, Harbin Institute of Technology, Harbin, PR China

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

Article history: As an attempt to tackle the problem of low strength and poor relative density of carbon nanotube (CNT)/
Received 7 January 2020 wood-plastic composites (WPC) manufactured by selective laser sintering (SLS), microwave treatment
Received in revised form 18 February 2020 was utilized to post-treat the SLS parts for the first time. The effects of microwave treatment on bending
Accepted 20 February 2020
properties and microstructure of CNT/pine wood powder/polyether sulfone (PES) composites by SLS were
Available online 21 February 2020
investigated. The results show that microwave treatment for less than 60 s can improve the bending
strength of CNT/WPC by 4.2–64.2% and it has little effect on SLS parts of both the WPC and its PES matrix.
Keywords:
This maybe because CNT under microwave irradiation can release intense heat and transfer it to the PES
Microwave treatment
Selective laser sintering (SLS)
matrix around CNT, leading to PES’s remelting partially and then solidifying rapidly, which results in
Carbon nanotube (CNT) better interfacial bonding between CNTs, PES matrix and wood powder.
Composite materials Ó 2020 Elsevier B.V. All rights reserved.
Bending strength

1. Introduction
Selective laser sintering (SLS) is a rapid and accurate additive
manufacturing technique to fabricate three-dimensional parts
with complex structure and shape [1,2]. Compared with traditional
technology, it has great potential to manufacture complex and
low-volume parts more rapidly. Wood-plastic composite (WPC)
is a new SLS material composed of wood powder and preferably
thermoplastics, which has the advantages of low cost, anti-aging,
high dimensional and stability [3,4]. However, sintered parts of
WPCs cannot be widely utilized due to their weak physical and
mechanical properties. The mechanical properties of the WPC with
the addition of the carbon nanotubes (CNTs) are enhanced by over
50% in our previous work [5]. In addition to adding nanoparticles,
post-treatment is also an effective technique to improve the
mechanical properties of WPC by SLS. Wax penetration and resin
penetration are two of the most common post-treatment methods
for SLS parts of WPC at present [6]. However, wax penetration sig-
nificantly reduces the life of the printed product and as for resin
penetration it is hard to infiltrate sticky resin into SLS parts. In
addition, they require both complicated operation and long pro-
cessing time. Therefore, it is urgent to obtain a facile post-
treatment method for SLS parts of WPC. The microwave heating
⇑ Corresponding author at: College of Mechanical and Electrical Engineering,
Northeast Forestry University, Harbin, PR China (Y. Zhang).
E-mail address: yunhe.zhang@nefu.edu.cn (Y. Zhang).
has the advantages of low energy consumption, low cost, simple
process, etc. Moreover, spark discharges from conductors under
microwave irradiation is very interesting and useful. Shim et al.
reported tensile strength of CNT-PET fabricated via microwave
irradiation is enhanced about 16% compared to a pristine sample
[7]. Qu et al. demonstrated the tensile strength of BPs (non-
woven CNT membranes)/PE with microwave irradiation showed
1.6 times greater than that of BPs/PE [8].
In this work, microwave treatment was for the first time inves-
tigated as post-processing method for CNT/WPC by SLS. The effects
of time duration of microwave treatment on bending properties of
CNT/pine wood powder/PES composites by SLS were discussed in
detail.
2. Experimental
In this work, the pine wood powder (particle diameter range of
45–96 mm), polyether sulfone (PES, particle diameter range of
0–58 mm) were purchased as wood reinforcement and polymer
matrix of WPC. Multi-walled carbon nano-tubes (CNTs, average
diameter of 50 nm, a length of 5–10 mm, purity level was greater
than 95%) were added into the WPC. Pine powder and PES powder
were dried for 10 h in the thermostat at 102 and 55 , respectively.
The dried pine powder and PES at a ratio of 1:6 (by mass fraction)
with 0.1 wt% the carbon nanotubes (CNTs) were mixed for 2 min
with rotational speed of 700r/min by mechanical mixing using an
SHR50A high-speed mixer.

https://doi.org/10.1016/j.matlet.2020.127547
0167-577X/Ó 2020 Elsevier B.V. All rights reserved.
2 Y. Zhang et al. / Materials Letters 267 (2020) 127547
Fig. 1. A photograph of (a) PES; (b) Wood powder/PES; (c) CNT/Wood powder/PES
bending test specimen by SLS.
The test specimens were sintered by an AFS-360 rapid proto-
typing equipment, product of Beijing Longyuan Technology Ltd.,
(Beijing, China). Experimental parameters were set as follows: pre-
heat temperature: 83 , layer thickness of 0.1 mm, and internal
power of 13 W. The microwave post-treatment process of the sin-
tered test specimens was carried out by adopting a microwave
oven (power: 385 W, frequency: 2.45 GHz). In order to reduce
the experimental error, the specimens were placed at the same
position of the microwave oven glass tray. More details on raw
materials, equipment and composites preparation has been pre-
sented in the previous work [5].
The PES, wood powder/PES and CNT/wood powder/PES speci-
mens with dimensions of 80 mm  10 mm  4 mm according to
the GB/T9341-2008 were sintered for three-point bending test as
shown in Fig. 1. The tests were performed on a CMT5504 testing
machine of TMS System Ltd with a cross-head speed of 10 mm/
min. The bending strength was obtained from five replicates. The
micro-morphology of the fracture surface was observed by the
FEI Quanta 200 scanning electron microscope.
3. Results and discussion
The effect of microwave treatment on the bending strength of
PES, wood powder/PES and CNT/wood powder/PES is shown in
Fig. 2a (microwave treatment time is 2 s). The bending strength
of PES and wood powder/PES specimens before and after micro-
wave treatment were almost similar, while that of CNT/wood pow-
der/PES specimens increases by 44.2% upon microwave treatment.
This maybe because the wood powder and the polymer PES are
non-conductors, their temperatures are almost not changed under
microwave treatment for a short time in this case. Thus, micro-
Fig. 2. (a) Effect of microwave treatment on bending strength of PES, Wood powder/PES and CNT/Wood powder/PES specimens; (b) Effect of microwave treatment time on
bending strength of CNT/Wood powder/PES.
wave treatment has no obvious effect on PES and WPC. In contrast,
CNT is a good conductor, which can absorb and transfer energy.
To further determine the effect of microwave treatment time on
the bending properties of CNT/WPC prepared by SLS, specimens
processed by microwave treatment for different times were tested.
The results are shown in Fig. 2b. It can be seen that the bending
strength of the specimen processed by microwave treatment was
increased by 4.2–64.2%. The bending strength increased at first
and then decreased slowly with microwave treatment time
increasing. For a 10 s microwave treatment sample, the bending
strength reached a maximum value of 15.6 MPa. When microwave
treatment time was 30 s, the bending strength tended to be con-
stant, with a value of 10.2 MPa.
The laser-sintering process of the specimens containing PES,
wood powder and CNT before microwave treatment was demon-
strated in our previous research [5]. A binding mechanism named
Partial melting arose in the present materials [9]. The loose com-
posite powder here before laser-sintering consists of PES particles
and wood powder particles, which are both covered with a thin
film of CNTs. When the laser heat supplied to the mixed powder
particles, partially-moltent PES particles would form necks
between PES particles and wood powder particles as well as the
CNTs would be embedded into the molten PES. This way PES, wood
powder and CNT get bonded together using laser. The fracture
microstructure of the specimens before and after microwave treat-
ment is shown in Fig. 3. For PES and wood powder/PES specimens,
the number of pores decreased to some extent after microwave
treatment than before microwave treatment (Fig. 3a–d). For CNT/-
wood powder/PES specimens without processed microwave treat-
ment, a lot of bare wood powder, melted PES as well as plenty of
fracture voids can be observed (Fig. 3e). The number of bare wood
powder decreased and the degree of melting of PES increased, at
2 s of microwave treatment time (Fig. 3f). Here the CNTs act as a
heat source to release heat and transfer heat to the PES matrix
under microwave treatment, it turns out that PES at a short dis-
tance from the CNTs would be heated selectively to remelt and
embed CNTs in a short time, while the core of PES particles would
not melt. In that case, the interfacial bonding between PES and CNT
would be enhanced after microwave treatment. The partially-
melted PES particles bind the bare wood powder particles and
CNTs again to form a molten polymer bulge (Fig. 3g), which
enhances the interface bonding between adjacent particles of PES
and wood powder. It was shown that CNTs were pulled out from
PES matrix (Fig. 3h) when the specimen was loaded with external
force. This also demonstrated that the interfacial bonding between
CNT and PES was better through microwave treatment. Wang et al.
 Y. Zhang et al. / Materials Letters 267 (2020) 127547 3

Fig. 3. SEM image of fracture surface of (a) untreated PES specimen; (b) PES specimen treated by microwave for 2 s; (c) untreated wood powder/PES specimen; (d) wood
powder/PES specimen treated by microwave for 2 s; (e) untreated CNT/wood powder/PES specimen; (f) CNT/wood powder/PES specimen treated by microwave for 2 s; (g)
CNT/wood powder/PES specimen treated by microwave for 30 s; (h) melted PES wrapped CNTs of CNT/wood powder/PES specimen of 2 s microwave treatment; (i) polymer
bulge of CNT/wood powder /PES specimen treated by microwave for 2 s.

also reported the strong bonding between CNTs and polymers
resulted from microwave treatment [10]. It can be concluded that
the interfacial bonding between CNT, wood powder and PES rather
than porosity is a dominant factor affecting the mechanical proper-
ties of specimens in this work.
After microwave treatment for as long as 30 s, the porosity of
sintered parts was significantly reduced and the density was
higher (Fig. 3i). This suggests the increasing microwave treatment
time leads to less pores of the CNT/WPC SLS parts, higher density of
parts and larger area where the more CNTs are wrapped by the PES.
However, excessive microwave treatment time causes the contin-
uous exotherm of the carbon nanotubes, which might give rise to
overheat of PES matrix close to CNTs. Then the PES would melt,
flow and be degraded at high temperatures, thus the bending
strength of specimens were reduced. Similar experimental results
were reported in previous studies [7,11].
4. Conclusions
powder/PES went up by 4.2–64.2%. The bending strength increased
with the increase of treatment time until 10 s, and then decreased.
The mechanism could be as following, upon microwave treatment,
PES at a short distance from the CNTs would be heated selectively
to remelt and embed CNTs promptly, while the core of PES parti-
cles would not melt. Thus, the interfacial bonding between PES
and CNT would be enhanced, which results in better interfacial
bonding between adjacent particles of PES and wood powder.
The excessive heat might destroy the PES matrix and result in
bending strength decreasing.
CRediT authorship contribution statement
Yunhe Zhang: Supervision, Project administration, Writing -
review & editing. Yanhong Cui: Writing - original draft, Investiga-
tion, Validation. Sian Wang: Writing - review & editing. Xiwang
Zhao: Validation. Fanming Wang: Validation. Gaohui Wu:
Conceptualization.

In summary, the microwave treatment can be used as a facile
post-treatment method to enhance the mechanical properties of
CNT/WPCs parts fabricated by SLS technology. The bending
strength of PES and wood powder/PES parts did not change
distinctly under microwave treatment while that of CNT/wood
Declaration of Competing Interest
The authors declare that they have no known competing finan-
cial interests or personal relationships that could have appeared
to influence the work reported in this paper.
4 Y. Zhang et al. / Materials Letters 267 (2020) 127547
Acknowledgements
We would like to acknowledge the financial supports to this
work by the Science and Technology Innovation Foundation for
Harbin Talents (Grant No. 2017RAYXJ021) and the Postdoctoral
Science Foundation of Heilongjiang Province, PR China. (Grant
No. LBH-Q18004).
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