polymers

Article
Efficient and Precise Micro-Injection Molding of
Micro-Structured Polymer Parts Using
Micro-Machined Mold Core by WEDM
Qianghua Liao 1 , Chaolan Zhou 2, *, Yanjun Lu 2, * , Xiaoyu Wu 2 , Fumin Chen 2 and Yan Lou 2
1 School of Mechanical and Electrical Engineering, Shenzhen Polytechnic, Shenzhen 518055, China;
liaoqianghua@szpt.edu.cn
2 Guangdong Provincial Key Laboratory of Micro/Nano Optomechatronics Engineering, College of
Mechatronics and Control Engineering, Shenzhen University, Shenzhen 518060, China;
wuxy@szu.edu.cn (X.W.); 2172291706@email.szu.edu.cn (F.C.); susanlou121@163.com (Y.L.)
* Correspondence: luyanjun@szu.edu.cn (Y.L.); zhouchaolan_scut@163.com (C.Z.); Tel.: +86-755-86950053




Received: 28 July 2019; Accepted: 27 September 2019; Published: 29 September 2019


Abstract: In this paper, micro-structured polymer parts were efficiently and accurately fabricated by
micro-injection molding using a micro-structured mold core machined by wire electrical discharge
machining (WEDM). The objective was to realize low-cost mass production and manufacturing of
micro-structured polymer products. The regular micro-structured mold core was manufactured by
precise WEDM. The micro-structured polymer workpieces were rapidly fabricated by micro-injection
molding and the effects of the micro-injection molding process parameters on replication rate and
surface roughness of micro-structured polymers were systematically investigated and analyzed.
It is shown that the micro-structured polymer can be rapidly and precisely fabricated by the
proposed method. The experimental results show the minimum size machining error of the
micro-structured mold core and the maximum replication rate of micro-formed polymer were 0.394%
and 99.12%, respectively. Meanwhile, the optimal micro-injection molding parameters, namely, jet
temperature, melt temperature, injection velocity, holding pressure and holding time were 195 ◦ C,
210 ◦ C, 40 mm/min, 7 Mpa and 5 s, respectively. The surface roughness Ra at the groove bottom
and top of the micro-structured polymer workpieces achieved minimum values of 0.805 µm and
0.972 µm, respectively.

Keywords: micro-structure; polymer; micro-injection molding; mold; WEDM

1. Introduction
Surfaces with micro/nano features on polymer components have been widely used in optical
displays, microfluidic chips, cell and tissue cultures, and other roles [1–4]. For example, a distribution
expression of microprism was designed on the bottom surface of an integrated light guide plate (ILGP).
The simulation results showed that the luminance uniformities of the integrated backlight modules
(BLMs) were higher than 85% [1]. A microfluidic chip combining poly-DL-lactide (PLA) patterned
electrospun fibers with polydimethylsiloxane (PDMS) was successfully developed by lithography to
realize toxicity screening of nanoparticles [2]. A 3D artificial polymeric scaffold with sub-micrometer
spatial resolution was fabricated to promote cell growth and tissue expansion [3]. A lab-on-a-chip (LoC)
with polymer substrate was fabricated for the application of non-invasive and contactless mechanical
phenotyping of single cancer cells [4].
Due to its simple manufacturing process, high forming quality and low production cost,
micro-injection molding is suitable for mass production and manufacturing of micro-structured
polymers, and it is almost unlimited in the geometric shape of plastic parts. Therefore, it has become the

Polymers 2019, 11, 1591; doi:10.3390/polym11101591 www.mdpi.com/journal/polymers

Polymers 2019, 11, 1591 2 of 15

main molding process of micro-structured polymer [5–7]. For instance, the disposable optical stretcher
and microfluidic devices can be rapidly and precisely fabricated by micro-injection molding [8,9].
The micro features with a width of 5 µm and a depth of 15 µm were precisely replicated by micro
injection molding [10]. The square pillared array structures with the sizes of 40 nm in width and 107 nm
in height (aspect ratio > 2.5) were fabricated by micro injection molding [11]. The micro-structured
surfaces with high aspect ratio can be also successfully replicated by micro injection molding [12].
The feasibility and availability of the micro injection molding technique had been demonstrated
in the presented works. The forming quality and replication accuracy of micro-injection molded
polymer products mainly depend on the machining quality and accuracy of the micro-structured
mold core. The common micro-machining technologies of the micro-structured mold core include
electrochemical etching [13], laser machining [14] and micro cutting machining [15]. However, it
is difficult to simultaneously ensure the macroscopic shape accuracy and the surface quality of 3D
micro-structures at the micron scale.
It is known that wire electrical discharge machining (WEDM) [16–18] is suitable for machining
complicated micro-structures with micron sizes. For instance, micro-grooved structures with size less
than 100 µm were fabricated on the surface of Ti3 SiC2 ceramic by WEDM to improve hydrophobic
performance [17]. A micro ball-ended probe with the diameter of 97.6 µm and surface roughness
Ra of 0.7 µm was successfully fabricated by micro-WEDM [18]. However, it is relatively difficult to
machine regular microarray structures with high 3D microscopic shape accuracy. In order to obtain
high surface quality and shape accuracy, micro-structures with a size within 100 microns are only
processed by low-speed WEDM. Therefore, high-precision low-speed WEDM was proposed to fabricate
micro-structures on the surface of the mold core to realize efficient mass-production and manufacturing
of micro-structured polymer parts by micro-injection molding.
In addition to the machining quality and precision of the micro-structured mold core, the
micro-injection molding process parameters also affect the forming quality of micro-structured
products. Generally, micro-injection molding has five steps, namely, injecting, packing, holding,
cooling and demolding. Due to the tiny structural size and volume of micro-injection molded parts, it
is difficult to ensure the shape accuracy and surface quality of injection molded micro-structured parts
under macroscopic injection molding process conditions [19,20]. Therefore, in this work, the influences
of micro-injection molding process parameters on the micro-forming accuracy and surface quality of a
micro-structured polymer workpiece were systematically investigated.
In this paper, the efficient and precise WEDM was firstly used to machine rectangular microarray
structures on the surface of mold core. Then, the micro-injection molding technology was used to
rapidly fabricate micro-structured polymer parts. Next, the influences of injection molding process
parameters, such as jet temperature, melt temperature, injection velocity, holding pressure and holding
time on the shape accuracy and replication rate of micro-structured polymer were analyzed. Finally,
the process conditions of micro-injection molding were optimized.

2. Materials and Methods

2.1. Wire Electrical Discharge Machining (WEDM) of Mold Core with Micro-Structures
As a promising mold material, titanium silicon carbide (Ti3 SiC2 ) combines the properties of both
metal and ceramic, and has high strength, fracture toughness, good thermal stability and workability,
and good self-lubrication and demolding performance [21,22]. Commercial Ti3 SiC2 bulk was cut into a
rectangular block with a size of 15 mm × 15 mm × 5 mm and mounted on the worktable of a wire
electrical discharge machining machine (AP250LS, Sodick, Yokohama, Japan). The conductive Ti3 SiC2
mold core was regarded as the cathode and was immersed into dielectric oil (Glysantin G 48–24, BASF,
Ludwigshafen, Germany) (see Figure 1). An anodic brass wire electrode with diameter of 50 µm
was employed to fabricate regular micro-structures on the surface of the Ti3 SiC2 mold core. Figure 1
shows the processing schematic diagram and machining scene of the mold core using WEDM. The
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Polymers 2019, 11, 1591 3 of 15

94 a, groove depth h and groove spacing b, were all set as 100 µm (see Figure 1a). Gradually, the
Polymers 2019, 11, x FOR PEER REVIEW 3 of 15
95 rectangular
designed micro-arraystructure
micro-grooved structures with macroscopic
parameters, namely, length
grooveand thickness
width of 7depth
a, groove mm ×h and
1.6 mm were
groove
9496 successfully
spacing b, werefabricated
all set as on
100the
µm surface
(see of the
Figure mold
1a). by WEDM
Gradually, under
the the driving
rectangular of the
micro-array
a, groove depth h and groove spacing b, were all set as 100 µm (see Figure 1a). Gradually, the wire electrode
structures
9597 feeding
with
rectangular system
macroscopic along
lengthastructures
micro-array predesigned
and thickness machining
withof 7 mm × 1.6
macroscopicpath.
mm Finally,
were
length and the machined
successfully
thickness 7micro-structured
fabricated
of mm × on 1.6 the mold
mmsurface
were
9698 ofcore
the was
mold cleaned
by WEDM by alcohol
under three
the times
driving in
of an
theultrasonic
wire cleaning
electrode machine.
feeding system along
successfully fabricated on the surface of the mold by WEDM under the driving of the wire electrode a predesigned
97 machining
feeding path.along
system Finally, the machined
a predesigned micro-structured
machining mold core
path. Finally, the was cleaned
machined by alcohol three mold
micro-structured times
98 in anwas
core ultrasonic
cleanedcleaning
by alcoholmachine.
three times in an ultrasonic cleaning machine.

99
100 Figure 1. The processing schematic diagram of mold core machined by wire electrical discharge
99
101 machining (WEDM): (a) schematic diagram of WEDM; (b) machining scene.
100 Figure
Figure 1.
1. The
Theprocessing
processingschematic
schematicdiagram
diagramofofmold
moldcore
core machined
machined byby wire
wire electrical
electrical discharge
discharge
102
101 2.2machining
Micro-injection
machining(WEDM): molding
(WEDM):(a) of polymer
(a)schematic workpieces
schematic diagram
diagram of with
of WEDM; micro-structures
WEDM; (b)
(b) machining
machining scene.
scene.

103
102
2.2. Micro-Injection
Polypropylene
2.2 Micro-injection
Molding
molding (PP) of Polymer
particles
of polymer
Workpieces
(B310, with
workpieces
with Micro-Structures
Lotte Chemical Corporation, Seoul, Korea) were
micro-structures
104 employed as the polymer workpiece material. The
Polypropylene (PP) particles (B310, Lotte Chemical Corporation, density of the polymer particlewere
Seoul, Korea) material was 0.9
employed
105
103 asg/cm
3 . Its theoretical
thePolypropylene
polymer workpiece thermal
(PP) deformation
material.
particles The temperature
density
(B310, of the
Lotte and melting
polymer
Chemical particlepoint were
material
Corporation, 110Korea)
was
Seoul, °C and
0.9 167
g/cmwere °C,
3 . Its
106
104 respectively.
theoreticalas
employed thermal Before micro-injection
deformation
the polymer temperature
workpiece molding,
material.and differential
Themelting
densitypoint
of the scanning
were ◦ calorimetry
110 Cparticle
polymer ◦
and 167material (DSC 8000,
C, respectively.
was 0.9
107
105 PerkinElmer,
Before
g/cm 3. Its Wellesley,
micro-injection
theoretical thermal MA,
molding, USA) testing
differential
deformation of polymer
scanning
temperature particles
calorimetry
and was
(DSC
melting conducted.
8000,
point Figure
PerkinElmer,
were 110 °C and 2Wellesley,
shows
167 °C,the
108
106 DSCUSA)
MA, heating
respectively. testingcurve
Before of the polymer
of polymer particles.
particlesmolding,
micro-injection was DuringFigure
conducted.
differentialthe scanning
heating
2 showsprocess
the DSCinheating
calorimetry DSC,(DSC one
curve sharp
8000, of
109
107 endothermic peak
the polymer particles.
PerkinElmer, appeared
Wellesley,DuringMA, USA)at nearly
the heating 167.2 °C,
testing process which was
in DSC,
of polymer close
one sharp
particles to the melting
endothermic
was conducted. point of the
peak2appeared
Figure polymer.
shows the at
110
108 Therefore,
nearly
DSC 167.2 ◦in
heating C, this
which
curve work, thethe
of was jet to
close
polymertemperature
meltingand
theparticles. pointmelt
During temperature
of the
thepolymer. should
processbeinin
heating Therefore, set at work,
this
DSC, a one
temperature
the jet
sharp
111
109 higher thanpeak
temperature
endothermic 167.2
and melt°Ctemperature
appearedto guarantee
at nearly complete
should
167.2 be
°C,setmelting of close
polymer
at a temperature
which was particles
higher
to the thanbefore
melting ◦injection
167.2 of
point Cthe into the
to guarantee
polymer.
112
110 mold
Therefore, core.
complete melting of polymer
in this work, the jetparticles before and
temperature injection
melt into the mold should
temperature core. be set at a temperature
111 higher than 167.2 °C to guarantee complete melting of polymer particles before injection into the
112 mold core.

113
114 Figure
Figure 2. 2.The
Thedifferential
differential scanning
scanning calorimetry
calorimetry (DSC)
(DSC) heating
heating curve
curve ofof
thethe polymer
polymer particles.
particles.
113
115
114 Micro-structured polymer
Figure 2. The differential components
scanning can(DSC)
calorimetry be rapidly
heatingfabricated
curve of theby micro-injection
polymer particles. molding
116 technology using the micro-structured mold core machined by WEDM. Figure 3 shows the
115 Micro-structured polymer components can be rapidly fabricated by micro-injection molding
116 technology using the micro-structured mold core machined by WEDM. Figure 3 shows the
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Polymers 2019, 11, x FOR PEER REVIEW 4 of 15

Micro-structured polymer components can be rapidly fabricated by micro-injection molding
117 technology using
principle and the micro-structured
forming mold core machined
process of micro-injection by WEDM.
molding Figure 3 showspolymer.
of micro-structured the principle
The
118 and forming process of micro-injection molding of micro-structured polymer. The polymer
polymer particles were put into a micro-injection molding machine (Babyplast 6/10P, Cronoplast Sl, particles
119 were put into
Barcelona, a micro-injection
Spain). molding molding
The micro-injection machine (Babyplast
machine has 6/10P,
the Cronoplast
advantagesSl, ofBarcelona,
small size,Spain).
high
120 The micro-injection molding machine has the advantages of small size,
molding precision and high efficiency, and thus is more suitable for mass productionhigh molding precision and
and
121 high efficiency, and
manufacturing thus precision
of small is more suitable
polymer forparts.
mass As production and manufacturing
seen in Figure 3, in the whole of small precision
micro-injection
122 molding process, the polymer particles were first heated and plasticized, then injected particles
polymer parts. As seen in Figure 3, in the whole micro-injection molding process, the polymer into the
123 were
mold first
coreheated and the
through plasticized,
pouringthen injected
gate. After into the mold
pressure core through
holding, coolingtheand
pouring gate. After
demolding, the
124 rectangular microarray structures on the surface of the micro-structured mold core can the
pressure holding, cooling and demolding, the rectangular microarray structures on the surface of be
125 micro-structured
replicated on themold core can
surface be replicated
of the polymer on the surface
workpiece. of the polymer
Therefore, workpiece. Therefore,
the micro-structured polymerthe
126 micro-structured
workpieces were polymer workpieces
rapidly fabricated bywere rapidly fabricated
micro-injection molding.by micro-injection molding.

127
128 Figure
Figure 3.
3. The
The schematic
schematic diagram
diagram of
of micro-injection
micro-injection molding
molding of micro-structured polymer.

129 WeWefurther
furtherinvestigated
investigatedthe theeffects
effectsofofmicro-injection
micro-injection molding
molding process
process parameters
parameters on on the
the
130 micro-forming quality
micro-forming quality ofof molded
molded polymer
polymer workpieces. According to
workpieces. According to previous
previous experiments,
experiments, when when
131 the mold
the mold temperature
temperature was was set
set atat room
room temperature,
temperature, the the micro-structured polymer samples
micro-structured polymer samples can can be
be
132 well-formed [6], so the mold temperature was not considered as an injection
well-formed [6], so the mold temperature was not considered as an injection molding process molding process parameter
133 in this paper.
parameter in In order
this to simplify
paper. In ordertest times, five
to simplify common
test times, process parameters,
five common processnamely, jet temperature
parameters, namely,
134 (the heating temperature of nozzle), melt temperature (the temperature of the
jet temperature (the heating temperature of nozzle), melt temperature (the temperature of the meltmelt polymer entering
135 the cavity),
polymer injection
entering thevelocity, holding pressure
cavity), injection velocity, and holding
holding time, and
pressure wereholding
selectedtime,
and were
set according
selected
136 to the single factor testing method in the experiments. The micro-injection
and set according to the single factor testing method in the experiments. The micro-injection molding parameters
137 and corresponding
molding parameterslevels
and incorresponding
designed experiments
levels inare listed inexperiments
designed Table 1. Because one setinofTable
are listed process1.
138 parameters
Because onewere
set repeated
of processfour times, therewere
parameters wererepeated
in total 21four
sets times,
of micro-structured
there were inpolymer.
total 21Samples
sets of
139 corresponded to the
micro-structured 21 setsSamples
polymer. of micro-injection
corresponded molding
to theprocess
21 setsparameters shown in
of micro-injection Table 1.process
molding Under
140 each process parameter, ten micro-injection molded workpieces were
parameters shown in Table 1. Under each process parameter, ten micro-injection molded selected for testing in order to
141 reduce the experiment
workpieces were selected error
forastesting
muchin asorder
possible.
to reduce the experiment error as much as possible.

2.3. Measurement of Micro-Structured Mold Core and Polymer Workpieces

142 2.3 Measurement of micro-structured mold core and polymer workpieces
The Raman spectrum (LabRAM HR Evolution, Horiba Jobin Yvon, France) was employed to
143 Theshift
detect the Raman spectrum
in phase (LabRAM
constitutions HRmold
of the Evolution, Horiba
core before andJobin
afterYvon,
WEDM France) was employed
processing. to
The surface
144 detect the shift in phase constitutions of the mold core before and after WEDM processing.
topographies of micro-machined mold cores and micro-formed polymer workpieces were characterized The
145 surface topographies
by high-resolution of micro-machined
scanning mold cores
electron microscope (SEM,and micro-formed
Apreo polymer
S, FEI Company, workpieces
Hillsboro, were
OR, USA).
146 characterized by high-resolution scanning electron microscope (SEM, Apreo S, FEI Company,
The 3D topographies and section profile curves of micro-structured mold cores and polymer workpieces
147 Hillsboro,
were OR,by
captured USA). The 3D topographies
non-contact andmicroscope
3D laser scanning section profile curves
(VK-250, of micro-structured
Keyence, Osaka, Japan).mold cores
Since the
148 and polymer workpieces were captured by non-contact 3D laser scanning microscope
top and bottom of the workpiece and mold core were not absolutely horizontal, the surface roughness (VK-250,
149 Keyence, Osaka, Japan). Since the top and bottom of the workpiece and mold core were not
150 absolutely horizontal, the surface roughness of Ra was uniformly used to evaluate the surface
151 qualities of machined mold core and formed polymer workpieces. Through the measured
Polymers 2019, 11, 1591 5 of 15

of Ra was uniformly used to evaluate the surface qualities of machined mold core and formed polymer
workpieces. Through the measured micro-grooved profile curves, the groove width, groove depth and
groove spacing of mold cores and polymer surfaces could be obtained. The presented experimental
results including the micro-groove size parameters and surface roughness Ra were the average values
of five measurements.

Table 1. The micro-injection molding parameters and corresponding levels in designed experiments.

Jet Melt
Injection Velocity Holding Pressure Holding Time
No. Temperature Temperature
V (mm/s) F (Mpa) t (s)
T 1 (◦ C) T 2 (◦ C)
1 185 210 40 7 5
2 190 210 40 7 5
3 195 210 40 7 5
4 200 210 40 7 5
5 205 210 40 7 5
6 195 200 40 7 5
7 195 205 40 7 5
8 195 215 40 7 5
9 195 220 40 7 5
10 195 210 30 7 5
11 195 210 35 7 5
12 195 210 45 7 5
13 195 210 50 7 5
14 195 210 40 5 5
15 195 210 40 6 5
16 195 210 40 8 5
17 195 210 40 9 5
18 195 210 40 7 3
19 195 210 40 7 4
20 195 210 40 7 6
21 195 210 40 7 7

3. Results and Discussions

3.1. Phase Constitutions of the Micro-Structured Mold Core Surfaces

Figure 4 shows the Raman spectra of the unprocessed and micro-structured Ti3 SiC2 mold core
surface. The spectra of the unprocessed surface had three sharp peaks at 223 cm−1 , 623 cm−1 and
675 cm−1 , and one broad peak at 276 cm−1 , which correctly corresponded to the E2g, A1g, E1g, and
A1g modes of Ti3 SiC2 , respectively [23], indicating that the major phase on the surface was Ti3 SiC2 .
Compared with the unprocessed surface, the micro-structured surface exhibited a wavier spectrum,
especially for the vibrational modes ranging from 450 cm−1 to 750 cm−1 , which indicated the existence
of titanium carbide [24]. The vanishing peak at 276 cm−1 , accompanied with the appearance of two
broad peaks at 1365 cm−1 and 1586 cm−1 , reflected the decreasing content in Ti3 SiC2 and increasing
disordered carbon [25]. Compared with the peaks assigned to Ti3 SiC2 , the peaks assigned to the
impurity were relatively lower than the former, indicating that the decomposition of Ti3 SiC2 on the
micro-structured surface was limited. Therefore, the chemical composition of the Ti3 SiC2 mold core
surface was hardly affected by electrical discharge machining.
 Polymers 2019, 11, x FOR PEER REVIEW 6 of 15
Polymers 2019, 11, 1591 6 of 15
Polymers 2019, 11, x FOR PEER REVIEW 6 of 15

171
172
171 Figure 4. The Raman spectra of the unprocessed and micro-structured Ti3SiC2 mold core surface.
Figure 4. The Raman spectra of the unprocessed and micro-structured Ti3 SiC2 mold core surface.
172
173 Figure 4. The Raman spectra of the unprocessed and micro-structured Ti3SiC2 mold core surface.
3.2 Topographies
3.2. Topographies and
and section
Sectionprofile
Profilecurves
Curvesofofmicro-structured
Micro-Structuredmold
Moldcore surfaces
Core Surfaces

173
174 Figure
Figure5 5shows
3.2 Topographies thethe
SEM
and section
shows photos
profile
SEM of the
curves
photos micro-structured
ofofmicro-structured mold
mold
the micro-structured corecore surface.
surfaces
mold As seen As
core surface. from Figure
seen from 5,
175 the regular micro-structured structures were successfully machined on the surface
Figure 5, the regular micro-structured structures were successfully machined on the surface of the of the mold core
174
176 by
mold Figure
WEDM.
core by 5 WEDM.
shows
Figure the
5b is anSEM photos
amplified
Figure 5b of
version
is an theofmicro-structured
amplified Figure 5a. As
version of shownmoldin
Figure 5a.core
As surface.
Figure inAsFigure
5b, a certain
shown seen from
number
5b, a
175
177 Figure
of small5, the regular
pores and micro-structured
microvilli produced structures
by the were successfully
decomposition of Timachined
3 SiC 2
certain number of small pores and microvilli produced by the decomposition of Ti3SiC2 into TiCinto on the
TiC and surface of
disorderedthe
176
178 mold
carbon core
[24] by
wereWEDM. Figure
distributed on 5b
theis an
grooveamplified
top and version
bottom, of Figure
which were 5a.
and disordered carbon [24] were distributed on the groove top and bottom, which were in in As shown
accordance in
withFigure
the 5b,
resultsa
177
179 certain
of the number
Raman of small
spectrum. pores
Comparedand microvilli
with the produced
groove top, by
the the
bottomdecomposition
had a more
accordance with the results of the Raman spectrum. Compared with the groove top, the bottom had of Ti
uniform 3SiC 2 into TiC
distribution
178
180 and
of disordered
pores
a more uniform carbon
and microvilli [24] of
because
distribution were distributed
electrical
pores erosion
and on the
mainly
microvilli groove
occurred
because intop
theand
electrical edge bottom,
regions
erosion which
of
mainly were top
theoccurred
groove in
in
179
181 accordance
during the with the
machining results of
process. the Raman spectrum. Compared
the edge regions of the groove top during the machining process. with the groove top, the bottom had
180 a more uniform distribution of pores and microvilli because electrical erosion mainly occurred in
181 the edge regions of the groove top during the machining process.

182
183
182 Figure 5.
Figure 5. SEM
SEM photos
photos of
of the
the micro-structured mold core
micro-structured mold core surface:
surface: (a)
(a) surface
surface topography of machined
topography of machined
184 mold core; (b) the magnified
magnified version
version of
of Figure
Figure 5a.
5a.
183 Figure 5. SEM photos of the micro-structured mold core surface: (a) surface topography of machined
184
185 Figure
mold
Figure
6 shows
core;
6 (b) thethe
shows
3D topographies
magnified and section
version of Figure
the 3D topographies and5a.
profile curves of the micro-structured mold core
section profile curves of the micro-structured mold
surface. Table 2 shows the surface roughness Ra and groove size parameters of the designed and
186 core surface. Table 2 shows the surface roughness Ra and groove size parameters of the designed
185
187 machined
Figure
and machined
micro-structured
6 shows the 3Dmold
micro-structured
cores. Asand
topographies
mold cores.
seensection
from Table 2, the
As seen profile
from Table
micro-machined
curves 2,ofthe
groove width
themicro-machined
micro-structured molda1 ,
groove
186
188 groove
core
width surface.
a1, groove
h1 and
depthTable 2 groove
shows
depth
spacing
the
h1 and
b1 were
surface
groove
almost in
roughness
spacing b1 Rwere
accordance
a and grooveinsize
almost
withparameters
the designed
accordance with of micro-groove
the
the designed
designed
187
189 sizes.machined
and The machined width error, depth
micro-structured mold error
cores.andAs spacing
seen error Table
from were 0.317
2,
micro-groove sizes. The machined width error, depth error and spacing error were 0.317 µm,
µm,
the 0.399 µm and 0.465
micro-machined µm,
groove
0.399
188
190 respectively.
width
µm and
The machined
a1,0.465
grooveµm,depth h1 arc
andcurve
respectively.
at the
groove
The
grooveb1bottom
spacing
machined were at
arc curve
side caninbeaccordance
almost observed onwith
the groove bottom side
the contour
canthe
of the
be designed
observed
189
191 micro grooves,sizes.
micro-groove and was
The mainly
machined attributed
width to the depth
error, cycloidal cross-section
error and spacingof error
the brass
on the contour of the micro grooves, and was mainly attributed to the cycloidal cross-section of wereelectrode,
0.317 leading
µm, 0.399
the
190
192 to
µm the
and existence
0.465 µm,of machining
respectively. error.
The The surface
machined arc roughness
curve at R
the a of the
groove groove
bottom top
brass electrode, leading to the existence of machining error. The surface roughness Ra of the groove
and
side can bottom
be of the
observed
191 micro-structured
on the contour of mold core machined
the micro grooves, andby WEDM
was mainly wereattributed
1.354 µm and 1.476
to the µm, respectively.
cycloidal cross-section of the
192 brass electrode, leading to the existence of machining error. The surface roughness Ra of the groove
 Polymers 2019, 11, x FOR PEER REVIEW 7 of 15

Polymers 2019, 11, 1591 7 of 15

193 top and bottom of the micro-structured mold core machined by WEDM were 1.354 µm and 1.476
194 µm, respectively.

195
196 Figure
Figure 6.
6. 3D
3D topographies
topographies and
and section
section profile
profile curves
curves of
of micro-structured
micro-structured mold
mold core surface.
core surface.

Table 2. The surface roughness and groove size parameters of the machined micro-structured mold core.
197 Table 2. The surface roughness and groove size parameters of the machined micro-structured mold
198 core. Spacing Ra of Groove Ra of Groove
Sample Width a1 (µm) Depth h1 (µm)
b1 (µm) Top (µm) Bottom (µm)
Width a1 Depth h1 Spacing Ra of groove top Ra of groove bottom
Sample
Machined mold (µm)
99.683 (µm)
99.601 b1 (µm)
100.465 (µm) 1.354 (µm)
1.476
core
Machined mold
99.683 99.601 100.465 1.354 1.476
core
According to the measured section profile curves before and after WEDM, the relative machining
199 According
errors to the measured
of the micro-structured moldsection profilerelative
core, namely, curveswidth
before and∆aafter
error WEDM,
m , relative theerror
depth ∆hm
relative
200 machining
and relativeerrors oferror
spacing ∆bm can be obtained
the micro-structured mold core,
by the namely,three
following relative width error Δam, relative
equations:
201 depth error Δhm and relative spacing error Δbm can be obtained by the following three equations:
∆am = (|a − a1 |/a) × 100% (1)
Δam=(|a–a1|/a)×100% (1)
∆bm = (|b − b1 |/b) × 100% (2)
Δbm=(|b–b1|/b)×100% (2)
∆hm = (|h − h1 |/h) × 100% (3)
Δhm=(|h–h1|/h)×100% (3)
By calculating the average value of the three relative machining errors, the average size machining
error of WEDM εm can be obtained by the following formula:
202 By calculating the average value of the three relative machining errors, the average size
203 machining error of WEDM εm can be εobtained
m = (∆amby + ∆b + ∆hm )/3 formula:
themfollowing (4)

After calculation by the above equations,

εm=(Δathe size
m+Δb machining
m+Δh m)/3 error εm of the micro-structured
(4)
mold core using WEDM was as low as 0.394%. Therefore, the regular micro-structured mold core can
204 be precisely machined
After calculation bybythe
WEDM,
above which was beneficial
equations, to produceerror
the size machining injection
εm ofmolded polymer parts
the micro-structured
205 with high
mold coreforming quality.was as low as 0.394%. Therefore, the regular micro-structured mold core
using WEDM
206 can
3.3. be precisely and
Topographies machined
Section by WEDM,
Profile Curveswhich was beneficialPolymer
of Micro-Structured to produce injection molded polymer
Surfaces
207 parts with high forming quality.
After the micro-injection molding experiments in Section 2.2 were implemented, 21 sets of
208 micro-structured
3.3 polymer
Topographies and section samples wereofobtained.
profile curves In orderpolymer
micro-structured to distinguish
surfaces the molding quality under
different injection molding process parameters, the sample with the best molding quality (experiment
209 After the micro-injection molding experiments in Section 2.2 were implemented, 21 sets of
No. 3 in Table 1), as well as five groups of test samples with the worst molding quality corresponding
210 micro-structured polymer samples were obtained. In order to distinguish the molding quality
to five process parameters were selected. The selected micro-formed polymer Samples 5, 6, 11, 17 and
211 under different injection molding process parameters, the sample with the best molding quality
25 were obtained when changing one process parameter and maintaining the other parameters, which
212 (experiment No. 3 in Table 1), as well as five groups of test samples with the worst molding quality
corresponded to jet temperature, melt temperature, injection velocity, holding pressure or holding
213 corresponding to five process parameters were selected. The selected micro-formed polymer
time, respectively. Figure 7 shows the SEM photos of the selected micro-injection molded polymer
Polymers 2019, 11, 1591 8 of 15

samples. It can be observed that the rectangular micro-array structures on the surface of the molded
polymer samples were roughly in accordance with that of the machined mold core (see Figure 5). It is
shown that micro-features on the surface of the micro-structured mold cores machined by WEDM
were successfully replicated on the micro-formed polymer surfaces, which indicated that the molten
polymer almost entirely filled into the micro-structures on the mold core surface. According to the
SEM topographies shown in Figure 7, the surface of Sample 3 (see Figure 7a) had the least adhesive
polymer debris compared with other samples (see Figure 7b–f). The SEM photo on the left is a larger
version of the photo on the right for a sample. It is found that the rectangular groove bottom surface
had better forming quality than the one of the groove top for all polymer samples. This is because the
surface quality of the groove top and groove bottom of injection molded polymer workpieces mainly
depends on the surface quality of the groove bottom and groove top of the micro-structured mold
core, respectively. Because the groove top surface of the mold core had been polished in advance, the
surface roughness Ra of the unprocessed groove top of the mold core was less than that of the groove
bottom machined by WEDM (see Table 2). Compared with the groove bottom surface, the surface
at the groove top of the micro-structured mold core was smoother, leading to smoother surfaces of
polymer samples at groove bottom against groove top.
In addition, it is also seen that there was significant residual cohesive polymer debris on the
surface of the groove top for all micro-formed polymer samples. This is because the polymer materials
shrank and deformed after heating and cooling in the micro-injection molding process. Therefore, the
micro-groove of the micro-structured mold core cannot be completely filled with molten polymers.
Furthermore, it is found that the residual melted polymer debris on the groove top surface of Sample
3 (see Figure 7a) was the least compared to other samples (see Figure 7b–f). It is clearly observed
that the size and number of cohesive polymers on the surface of different samples corresponding to
different micro-injection molding process parameters were different (see Figure 7b–f). It is confirmed
that the micro-forming quality of micro-structured polymer was related to the micro-injection molding
process parameters. Therefore, it is necessary to choose appropriate micro-injection molding process
parameters in the production and manufacturing of micro-structured polymer parts.
Figure 8 shows the 3D topographies and section profile curves of selected micro-injection molded
polymer samples. The selected samples shown in Figure 8 correspond to those shown in Figure 7.
The results of 3D topographies and profiles shown in Figure 8 further confirm the SEM results shown
in Figure 7. Compared with other samples, Sample 3 had a relatively smooth surface at groove
tops and bottoms. Through the measured profile curves of rectangular micro-groove structures, the
micro-structure size parameters of micro-injection molded polymer workpieces including groove
width a2 , groove depth h2 and groove spacing b2 can be acquired. The surface roughness Ra of groove
bottom and groove top on micro-formed polymer surfaces can be also obtained.
 Polymers 2019, 11, 1591 9 of 15

Polymers 2019, 11, x FOR PEER REVIEW 9 of 15

255
256 FigureFigure 7. SEM
7. SEM photos
photos of the
of the selectedmicro-structured
selected micro-structured polymer
polymersamples:
samples:(a) (a)
Sample 3; (b)
Sample 3;Sample 5;
(b) Sample 5;
257 (c) Sample
(c) Sample 6; (d)6;Sample
(d) Sample
11;11;
(e)(e) Sample17;
Sample 17;(f)
(f)Sample
Sample 25.
25.
 Polymers 2019, 11, 1591 10 of 15
Polymers 2019, 11, x FOR PEER REVIEW 10 of 15

258
259 Figure
Figure 8. 3D topographies
8. 3D topographiesofofthe
themicro-structured
micro-structuredpolymer
polymersamples:
samples:
(a)(a) Sample
Sample 3; (b)
3; (b) Sample
Sample 5;
5; (c)
260 (c) Sample
Sample 6; (d)
6; (d) Sample
Sample 11;11;
(e)(e) Sample
Sample 17;17;
(f) (f) Sample
Sample 25.25.

261 Table
Table 3 shows
3 shows thethe surfaceroughness
surface roughnessand andmicro-structure
micro-structuresize sizeparameters
parametersof ofmolded
molded polymer
polymer
262 workpieces. As seen from Table
workpieces. Table 3, 3, the
the surface
surfaceroughness
roughnessRRaa on the surface of the groovegroove bottom
bottom was
263 less than
less thanthat
thatononthethe surface
surface of groove
of the the groove topallfor
top for all micro-structured
micro-structured polymer polymer
samples.samples. This is
This is because
264 because the surface quality at the groove bottom of micro-structured polymer
the surface quality at the groove bottom of micro-structured polymer mainly depends on the surface mainly depends on
265 the surface
quality at thequality
grooveattop theofgroove
the mold topcore.
of the mold core.
Moreover, Moreover,
comparing thecomparing the surface
surface roughness Ra ofroughness
the mold
266 R of the mold core shown in Table 2 with polymer workpieces shown in Table
core shown in Table 2 with polymer workpieces shown in Table 3, it is found that the surface roughness
a 3, it is found that the
267 surface
of roughness
polymers was lessofthan
polymers
that ofwas less than
the mold core.that
Theof the mold
reason may core. The
be that thereason may be did
melt polymer thatnot
thefill
melt
all
268 polymer
peaks anddid not due
valleys fill to
alltrapped
peaks air,
andresulting
valleys in due to trapped
a better air, According
roughness. resulting in a better
to the resultsroughness.
of Table 3,
269 According
in the process to of
themicro-injection
results of Table 3, in the
molding, theprocess
average ofwidth
micro-injection molding,
error, average depththeerror average width
and average
270 error, average
spacing error weredepth1.277error
µm,and average
1.158 µm and spacing
1.050 µm,errorrespectively.
were 1.277 Because
µm, 1.158theµm and 1.050
designed µm,
original
271 respectively.
theoretical Because
sizes the designed original
of micro-structures were 100theoretical sizes of micro-structures
µm, the micro-forming accuracy ofwere 100 µm, the
micro-structured
272 micro-forming
polymer was only accuracy
about 1%. of micro-structured
Moreover, under polymer was only aboutmolding
different micro-injection 1%. Moreover,
parameters, under different
the groove
273 micro-injection
size parameters and molding
surface parameters,
roughness of the groove size parameters
micro-structured and surface
polymer workpieces wereroughness
different (see of
274 micro-structured polymer workpieces were different (see Table 3). Therefore,
Table 3). Therefore, it is necessary to investigate the effects of micro-injection molding parameters on it is necessary to
275 investigate the effects of micro-injection molding parameters
the micro-forming quality and replication precision of micro-structured polymer. on the micro-forming quality and
276 replication precision of micro-structured polymer.

277

278

279
Polymers 2019, 11, 1591 11 of 15

Table 3. The surface roughness and groove size parameters of micro-structured polymer workpieces.

Depth h2 Spacing b2 Ra of Groove Bottom Ra of Groove Top

No. Width a2 (µm)
(µm) (µm) (µm) (µm)
1 100.44 100.967 98.164 0.864 0.996
2 99.069 101.469 98.278 0.871 1.028
3 100.339 101.183 98.503 0.805 0.972
4 98.090 100.667 100.981 0.903 1.166
5 97.087 100.932 100.016 0.943 1.286
6 97.805 100.534 101.451 1.202 1.503
7 98.086 99.998 101.229 1.153 1.396
8 99.414 101.665 98.140 0.874 1.065
9 98.253 100.006 100.986 0.929 1.269
10 100.009 101.48 101.581 0.962 1.287
11 100.05 101.965 98.943 0.804 0.976
12 99.925 101.764 100.834 0.817 0.955
13 98.515 102.109 100.161 0.948 1.241
14 98.198 100.111 101.439 1.163 1.422
15 97.441 99.720 100.570 1.329 1.459
16 98.231 101.845 98.972 1.118 1.326
17 99.185 101.487 101.915 1.267 1.398
18 98.299 101.786 99.534 0.860 1.035
19 98.870 102.251 99.934 0.856 1.016
20 100.909 101.483 100.076 0.822 1.003
21 98.472 99.670 101.289 1.120 1.411

3.4. Effects of Micro-Injection Molding Parameters on Replication Rate of Micro-Structured Polymer

According to the measured section profile curves before and after micro-injection molding and the
data results shown in Table 3, the relative micro-forming errors of micro-structured polymer, namely,
relative width error ∆aw , relative depth error ∆hw and relative spacing error ∆bw can be calculated
as follows:
∆aw = (|b2 − a1 |/a1 ) × 100% (5)

∆bw = (|a2 − b1 |/b1 ) × 100% (6)

∆hw = (|h2 − h1 |/h1 ) × 100% (7)

The replication precision of micro-features on the mold core surface, which decided the forming
quality of micro-injection molding, can be evaluated by the filling rate. In this work, the replication
rate was the main output target to evaluate the replication quality of molded polymer workpieces. The
replication rate was defined as the ratio of each micro-structural volume of micro-injection molded
part to the micro-structural volume of the mold core. As mentioned in the previous experiment, the
thickness of both micro-structured polymer and mold core was 1.6 mm. Therefore, the replication
rate was only related to the average depth, width and spacing of the micro-structure sizes. The
micro-forming accuracy of micro-injection molding εw can be computed by the following equation:

εw = (∆aw + ∆bw + ∆hw )/3 (8)

Therefore, the replication rate of micro-injection molding γ can be obtained by the

following formula:
γ = 100% − εw (9)

Based on the above equations, the effects of micro-injection molding parameters on the replication
rate of micro-structured polymers are depicted in Figure 9. As seen from Figure 9, when the
micro-injection molding parameters, namely, jet temperature T1 , melt temperature T2 , injection velocity
V, holding pressure F and holding time t were 195 ◦ C, 210 ◦ C, 40 mm/min, 7 Mpa and 5 s, respectively,
Polymers 2019, 11, 1591 12 of 15

the replication rate γ of micro-formed polymer reached a maximum value of 99.12%. There was no
significant change in the replication rate when the jet temperature increased. The replication rate
was ranged from 98.89% to 99.12% with the change of jet temperature. The replication rate achieved
a maximum value of 99.12% until the jet temperature increased to 195 ◦ C (see Figure 9a). With the
continual increase of jet temperature, the replication rate rapidly decreased. The reason may be that
too high jet temperature affects the flow rate and injection volume of melted polymer, leading to
incomplete injection filling. Figure 9b shows the effect of melt temperature on the replication rate
of polymer workpieces. The replication rate first dramatically increased, and then slowly decreased
with the increase of melt temperature. The range of replication rate was 98.78% to 99.12% with the
change of melt temperature. This indicated that the melt temperature cannot be too high or too low.
It would produce uneven forming of melt polymer if the melt temperature was too low. A melt
temperature that is too high would cause excess shrinkage in cooling and solidification. The effect
of injection velocity on the replication rate is shown in Figure 9c. The replication rate first increased,
and then rapidly decreased with the increase of injection velocity. The replication rate was ranged
from 98.89% to 99.12% with the change of injection velocity. As the injection velocity ranged from
35 mm/s to 45 mm/s, the variation of the replication rate was insignificant. This indicated that the
proper injection velocity was conducive to sufficient filling and replication of melted polymer in the
process of micro-injection molding. The possible reasons are that it would affect the flow rate of melted
polymer if the injection velocity was too slow, leading to incomplete filling for micro-structure features.
If the injection velocity was too fast, it would cause uneven filling between melted polymer and the
mold core. In Figure 9d, the highest replication rate only can be achieved under the holding pressure
of 7 MPa, while a holding pressure higher or lower than 7 MPa would lead to a sharp decrease in the
replication rate. This illustrated that the holding pressure had a large influence on micro-forming
quality and replication rate. The replication rate was ranged from 98.74% to 99.12% with the change of
holding pressure. Figure 9e shows the effect of the holding time on the replication rate of polymer
workpieces. Although the optimal holding time was 5 s, the replication rate smoothly increased when
the holding time ranged from 3 s to 6 s, and then prominently decreased when the holding time
exceeded 6 s. The replication rate was ranged from 98.81% to 99.12% with the change of holding time.
Compared with injection velocity and jet temperature, the effects of the melt temperature, holding
pressure and holding time on the replication rate of micro-structured polymer were more significant in
the process of micro-injection molding.

3.5. Effects of Micro-Injection Molding Parameters on Surface Quality of Micro-Structured Polymer

The surface roughness Ra at the groove top and bottom of micro-structured polymers was obtained
by measured section profiles (see Table 3). Figure 10 shows the effects of micro-injection molding
parameters on surface roughness Ra . It is shown that the surface roughness at the groove top was larger
than that at the groove bottom under the same micro-injection molding parameters. The increasing or
decreasing trends of surface roughness at the groove top and bottom with the changes of micro-injection
molding parameters were consistent. As seen from Figure 10, when the micro-injection molding
parameters, namely, jet temperature T1 , melt temperature T2 , injection velocity V, holding pressure F
and holding time t were 195 ◦ C, 210 ◦ C, 40 mm/min, 7 Mpa and 5 s, respectively, the surface roughness
Ra at the groove bottom of the micro-structured polymer achieved a minimum value of 0.805 µm.
Meanwhile, the replication rate reached the maximum value of 99.12% (see Figure 9).
 Polymers 2019, 11, x FOR PEER REVIEW 13 of 15
Polymers 2019, 11, 1591 13 of 15
Polymers 2019, 11, x FOR PEER REVIEW 13 of 15

347
347
348 Figure 9. The effects of micro-injection molding parameters on replication rate γ: (a) jet temperature
348
349 Figure 9. The effects of micro-injection molding parameters on replication rate γ: γ: (a) jet temperature
T1; (b) melt temperature T2; (c) injection velocity V; (d) holding pressure F; (e) holding time t.
349 T 1 ; (b) melt temperature T 2 ; (c) injection velocity V; (d) holding pressure F; (e) holding
T1; (b) melt temperature T2; (c) injection velocity V; (d) holding pressure F; (e) holding time time t.t.

350
350
351 Figure 10.
Figure 10.The
The effects
effects of micro-injection
of micro-injection molding molding parameters
parameters onroughness
on surface surface roughness Ra: (a) jet
Ra : (a) jet temperature
351
352 Figure
temperature
T 1 ; (b) 10. temperature
melt The
T effects
1; (b) melt of
T 2 ; micro-injection
temperature
(c) T
injection molding
2;velocity
(c) injection
V; parameters
velocity
(d) holdingV; onholding
(d) surface
pressure F; (e) roughness
pressure
holding F;
time Rt.a:holding
(e) (a) jet
352
353 temperature
time t. T1; (b) melt temperature T2; (c) injection velocity V; (d) holding pressure F; (e) holding
353 time surface
The t. roughness at the groove top and bottom first slowly decreased, then dramatically
354 The with
increased surface
theroughness
increase ofatjetthe groove top(see
temperature andFigure
bottom10a).
firstThis
slowly decreased,
is because a jetthen dramatically
temperature that
354
355 was Thehigh
increased
too surface
with theroughness
was increase
not ofatjetthe
conducive togroove
temperature
the flowtopofand
(see bottom
Figure
molten firstThis
10a).
polymer, slowly decreased,
is because
leading a jet
to the then dramatically
temperature
rapid reductionthat
in
355
356 increased
was
replication with
too high the
ratewas increase
andnot ofinjet
conducive
increase temperature (see
to theroughness.
surface flow of Figure
molten 10a).
Figurepolymer, Thisleading
10b shows isthat
because a jet
to surface
the the temperature
rapid reduction
roughness that
in
first
356
357 was too high
replication
rapidly was not
rate andthen
decreased, conducive
increase to
in surface
increased the flow of
roughness.
with the molten
increasingFigurepolymer,
melt 10b leading
shows that
temperature. to the rapid
theindicated
This reduction
surface roughness in
that there first
was
357
358 replication
arapidly rate and
decreased,
large influence increase
of then in surface
increased with
melt temperature roughness.
on the Figure
increasing
surface 10b shows
meltIt temperature.
roughess. that
is seen that thethe surface
This roughness
indicated
surface first
that there
roughness first
358
359 rapidly
was decreased,
a large influencethen increased
of melt with theonincreasing
temperature melt temperature.
surface roughess. Thisthe
It is seen that indicated that there
surface roughness
359 was a large influence of melt temperature on surface roughess. It is seen that the surface roughness
Polymers 2019, 11, 1591 14 of 15

significantly decreased, then slowly increased with the increase of injection velocity (see Figure 10c).
This is because an injection speed that was too slow or too fast would cause the melted polymer to not
fully fill the micro-structured mold core. Figure 10d shows that the surface roughness first rapidly
decreased, then sharply increased with the increase of holding pressure. This indicated that the holding
pressure had a great influence on the surface roughness. It shows that the surface roughness first
slowly decreased, then greatly increased with the increase of holding time (see Figure 10e). As a result,
compared with injection velocity, jet temperature and holding time, the melt temperature and holding
pressure had greater influence on the surface roughness of micro-formed polymer.

4. Conclusions
The highly efficient and precise wire electrical discharge machining (WEDM) technology is
proposed to fabricate rectangular micro-grooved array structures on the surface of a mold core.
Micro-injection molding is employed to fabricate micro-structured polymers using a micro-structured
mold core machined by WEDM. The proposed fabrication method for micro-structured polymer parts
may be widely applied and developed due to its low manufacturing cost and possible mass production.
The main results are summarized as follows:
1. The regular micro-structures can be accurately processed on the surface of the mold core
by WEDM. The chemical compositions of the Ti3 SiC2 mold core surface are hardly changed in the
process of electrical discharge machining. The average size machining error of micro-structured
mold core using WEDM was 0.394%. The machined surface roughness Ra at the groove bottom of
micro-structured mold core was 1.476 µm.
2. The micro-forming quality of micro-structured polymer is related to the micro-injection molding
process parameters. In order to obtain the highest replication rate of 99.12% for micro-formed polymer,
the optimal micro-injection molding parameters, namely, jet temperature, melt temperature, injection
velocity, holding pressure and holding time are 195 ◦ C, 210 ◦ C, 40 mm/min, 7 Mpa and 5 s, respectively.
3. Compared with injection velocity and jet temperature, the effects of the melt temperature,
holding pressure and holding time on the replication rate of micro-structured polymer are more
significant. The melt temperature and holding pressure have significant influences on the surface
roughness of micro-formed polymer. The minimum surface roughness Ra at the groove bottom of
micro-structured polymer is 0.805 µm.

Author Contributions: Conceptualization, Y.L.(Yanjun Lu); Data curation, Y.L.(Yanjun Lu) and F.C.; Formal
analysis, C.Z.; Funding acquisition, Q.L., X.W., Y.L.(Yanjun Lu) and Y.L.(Yan Lou); Investigation, C.Z. and F.C.;
Methodology, Y.L.(Yanjun Lu); Supervision, X.W. and Y.L.(Yan Lou); Validation, C.Z.; Writing—original draft, C.Z.
and Y.L.(Yanjun Lu); Writing—review & editing, Q.L. and Y.L.(Yanjun Lu)
Funding: This research was funded by the National Natural Science Foundation of China (grant numbers
51805334, 51575360 and 51675347), the Science and Technology Planning Project of Shenzhen City (grant number
JCYJ20170818114408837), the Science and Technology Planning Project of Guangdong Province (grant numbers
2016A040403043 and 2017A010102003), the major project for industrial technology of Guangzhou City (grant
number 201902010018), the Fundamental Research Funds for the Shenzhen University (grant number 2018031),
the Youth Projects for Creative Talents of Educational Commission of Guangdong Province (grant number
2015KQNCX009).
Conflicts of Interest: The authors declare no conflict of interest.

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