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materials
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Article
1
School of Mechanical Science and Engineering, Jilin University, Renmin Street 5988,
Changchun 130025, China; E-Mails: wzwu@jlu.edu.cn (W.W.);
gengpeng13@mails.jlu.edu.cn (P.G.); ligw1411@mails.jlu.edu.cn (G.L.);
zhaodi@mails.jlu.edu.cn (D.Z.)
2
Alan G. MacDiarmid Institute, College of Chemistry, Jilin University, Qianjin Street 2699,
Changchun 130012, China; E-Mail: zhanghaib@jlu.edu.cn
materials was similar. These results indicate that the mechanical properties of 3D-printed
polyether-ether-ketone (PEEK) are superior to 3D-printed ABS.
1. Introduction
2. Experimental Section
Mechanical properties of 3D-printed samples can be influenced by many factors, such as layer
thickness, raster angle, build orientations, fill pattern, air gap and model build temperature. Layer
thickness is the thickness of the layer deposited by the nozzle. Raster angle is the direction of raster
Materials 2015, 8 3885
Materials 2015, 8 5836
thickness is the thickness of the layer deposited by the nozzle. Raster angle is the direction of raster
with respect
with respect to
tothe
theloading
loadingdirection
directionofofstress,
stress,asas shown
shown in Figure
in Figure 1. Air
1. Air gapgap is distance
is the the distance between
between two
two adjacent
adjacent deposited
deposited filaments
filaments in the
in the same
same layer.
layer. Thenumber
The numberofofcontours
contoursisisthe
the number
number ofof filaments
filaments
initially deposited
initially deposited along
along the
the outer
outer edge.
edge.Bead
Beadwidth
widthis is
thethe
width of the
width filament
of the filamentdeposited by the
deposited 3D
by the
printer
3D nozzle.
printer nozzle.
work described
The work described herein
hereininvestigated
investigatedthe theinfluence
influenceofoflayer
layer thickness
thickness (LT)
(LT) andand raster
raster angle
angle (RA)(RA)
on
on the
the mechanical
mechanical properties
properties of PEEK
of PEEK samples
samples builtbuilt
by a by a custom-built
custom-built 3D printing
3D printing system.
system. SamplesSamples
with
with three
three rasterraster
anglesangles
(0,and
(0 , 30
3045and
45)three
) and and layer
three thicknesses
layer thicknesses (200,
(200, 300 300
and and
400 400were
m) m)built
werebybuilt
3D
by 3D printing
printing of PEEKofand PEEK
testedand tested for
for tensile, tensile, compressive
compressive and bending
and bending strengths. Thestrengths. The printing
printing parameters are
parameters
shown are shown
in Table 1. Buildinorientation
Table 1. Buildrefersorientation refers to
to the inclination of the
partinclination of part inwith
in a build platform a build platform
respect to X,
with
Y, respect
Z axis to X,
(side, flatY,
andZ up)
axis[18].
(side,Inflat
ourand up)samples
study, [18]. In grown
our study, samples
up along grown
Z axis and up
sat along
down Z flataxis and
during
sat down
the flatprocess.
building during the Fillbuilding
pattern process. Fill pattern
is the motion path ofisthe
the3D
motion pathmachines
printing of the 3D liquefier
printing head
machines
[19].
liquefierthe
During head [19]. process,
printing During the printing head
the liquefier process,
movetheback
liquefier headforming
and forth move back and forthstructure
a rectangular formingtoa
rectangular
fill the entirestructure
internal to fill the
portion ofentire
layer. internal
Air gap portion
is the gapof between
layer. Airtwo gapadjacent
is the gap between
rasters two layer.
on same adjacent
rasters on same layer.
Table 1. The printing parameters of polyether-ether-ketone (PEEK) 3D printing.
Table 1. The printing parameters of polyether-ether-ketone (PEEK) 3D printing.
Control Factors Fixed Factors
Factor Control Factors
Level Unit Factor Fixed FactorsValue Unit
Factor Level Unit Factor Value Unit
200
200 mm
mm Buildorientation
Build orientation Y-direction (Flat)
Y-direction (Flat) --
Layer thickness
Layer thickness 300
300 mm
mm Fillpattern
Fill pattern Line
Line --
400
400 mm
mm Air
Airgap
gap 00 mm
mm
00
Number
Numberof ofcontours
contours 22 - -
Raster
Raster angle
angle 30 Nozzle inner inner
Nozzle diameter 0.4 mm
30 0.4 mm
45 diameter
45
Materials 2015, 8 5837
Figure 2. Standard samples for mechanical tests. (a) Tensile samples; (b) Bending samples;
Figure 2. Standard samples for mechanical tests. (a) Tensile samples; (b) Bending samples;
(c) Compressive samples.
(c) Compressive samples.
TM
The experimental
The experimental samples
samples were were
mademade
from from
PEEKPEEK and ABS
and ABS plusTMplus -P430.
-P430. High-performance
High-performance PEEK PEEK
material
material was obtained from the Jilin University Special Plastic Engineering Research
was obtained from the Jilin University Special Plastic Engineering Research Co. Ltd. (Changchun, China), with Co. Ltd.
(Changchun, China), with a melting point of 334 C, a glass transition temperature of 143 C and
a melting point of 334 C, a glass transition temperature of 143 C and a melt index of 44 g/10 min.
a melt index of 44 g/10 min. PEEK samples were then built with a custom-built 3D printing system. In
PEEK samples were then built with a custom-built 3D printing system. In this printing machine, a stage
this printing machine, a stage platform moves in the X- and Y- axes, and a head including a nozzle tip
platform movesheater
and nozzle in themoves
X- and Y- axes,
along and awhile
the Z-axis, headfusing
including a nozzlematerial.
and depositing tip and ABS
nozzle heater moves
is inexpensive, hasalong
the Z-axis, while fusing
high mechanical and depositing
strength, and is widelymaterial. ABS
used in the 3D is inexpensive,
printing industry has
[20].high
ABSmechanical
plusTM-P430strength,
material and
TM
(Stratasys
is widely used Inc.,
in theEden
3D Prairie,
printingMN, USA) [20].
industry was used
ABSto plus
make ABS-P430samples. ABS
material is ideal for
(Stratasys building
Inc., Eden 3DPrairie,
MN, parts
USA)whenwascombined with uPrint
used to make ABSSE 3D Printers
samples. ABS (Stratasys
is idealInc.,
for Eden Prairie,
building 3DMN, partsUSA).
when ABS samples with
combined
uPrintwere
SE built with uPrint
3D Printers SE 3D Printers
(Stratasys usingPrairie,
Inc., Eden default building
MN, USA). parameters
ABS to obtain optimal
samples mechanical
were built with uPrint
properties. The SR-30 Soluble Support (synthetic thermoplastic polymer) was used as
SE 3D Printers using default building parameters to obtain optimal mechanical properties. The SR-30the support material.
The mechanical properties of PEEK and ABS materials are shown in Table 2. Testing of mechanical
Soluble Support (synthetic thermoplastic polymer) was used as the support material. The mechanical
properties of the raw materials were performed on samples manufactured by injection molding.
properties of PEEK and ABS materials are shown in Table 2. Testing of mechanical properties of the
raw materials Table 2. Mechanical
were performed on properties of PEEK and acrylonitrile
samples manufactured by injection butadiene
molding. styrene (ABS).
Factor PEEK ABS
Table 2. Mechanical properties of PEEK and acrylonitrile butadiene styrene (ABS).
Tensile Strength 100.0 MPa 37.0 MPa
Elastic Limit 72.0 MPa 31.0 MPa
Factor PEEK ABS
Compressive Strength 118.0 MPa 37.0 MPa
Compressive Modulus
Tensile Strength 3.8 GPa
100.0 MPa 2.3 GPa
37.0 MPa
Bending Strength
Elastic Limit 163.0
72.0 MPa
MPa 53.0 MPa
31.0 MPa
Bending Modulus
Compressive Strength 4.0 GPa
118.0 MPa 2.2 GPa
37.0 MPa
Compressive Modulus 3.8 GPa 2.3 GPa
Bending Strength 163.0 MPa 53.0 MPa
Bending Modulus 4.0 GPa 2.2 GPa
Materials 2015, 8 5838
The mechanical tests were carried out on an autograph universal materials testing machine, equipped
with a 50-kN load cell. To minimize experimental error, five samples were built and tested under identical
conditions for each mechanical test and the mean values were taken as the results. The samples were
performed according to the GB/T 16421-1996 Standard and the samples stretched at a strain rate of
1 mm/min. The three-point bending tests were performed according to the GB/T 9341-2008 Standard
with the loading rate of 2 mm/min, the span was 64 mm and the head of loading device was composed of
steel cylinders 10 mm in diameter. The compressive test was performed according to the GB/T1041-2008
Standard at a loading rate of 2 mm/min.
3.1. Influence of Layer Thickness and Raster Angle on Mechanical Properties of PEEK
Table 3 shows the practical mean values of mechanical tests for the 3D-printed PEEK samples. From
Table 3, it can be noted that the samples built with a 300-m layer thickness had the greatest strengths
in all mechanical tests. The strength of samples with a 400-m layer thickness decreased significantly.
We can also see that samples built with raster angles of 0 /90 had the greatest mechanical strengths.
Although the layer thickness had a great influence on tensile strength, it had little influence on bending
and compressive strengths. Because the compressive sample was cylindrical, there was no effect of the
raster angle.
Table 3. Mechanical properties in different layer thickness and different raster angles.
As indicated in Table 3, the tensile strengths of the PEEK samples were significantly affected by
the layer thickness and raster angle. In samples printed at raster angles of 0 /90 , the filaments were
oriented parallel to the load direction, producing the strongest samples. Similarly, in samples printed
in other orientations, there was a finite angle between the printed microstructural elements and the load
direction. The filaments were thus subjected to both tensile and shear stresses, leading to failure at low
tensile strength.
During compressive tests, the samples undergo pressure aligned in the axial direction and the adjacent
layers bear the shear stress because of the additive build up, which can cause the single layers to
slide along one another until the sample finally breaks. The compressive strength of printed samples
is significantly lower than that of injected materials because the printed samples are subject to flaws,
comprising both extensive pores that are initially squeezed out and weak interlayer bonding.
Materials 2015,
Materials
Materials 2015, 888
2015,
5839
3888
3888
Weak interlayer
Weak
Weak interlayer bonding
interlayer bonding is
bonding is responsible
is responsible for
responsible for aaa decrease
for decrease in
decrease in bending
in bending strength,
bending strength, which
strength, which can
which can cause
can cause welded
cause welded
welded
layers to
layers to delaminate. During printing,
delaminate. During printing, each
each new
new layer
layer will
will overlay
overlay the
the top
top ofof the
the previous
previous layer before
layer before
before
material solidification
material
material solidification from
solidification from the
from the melt occurs,
the melt
melt occurs, which
occurs, which leads
which leads to
leads to shrinkage
to shrinkage in
shrinkage in the previous
in the
the previous layer.
previous layer. The
layer. The residual
The residual
residual
stresses in
stresses
stresses in the
in the printed
the printed samples
printed samples resulting
samples resulting from
resulting from the
from the volume
the volume shrinkage
volume shrinkage were
shrinkage were examined
were examined to
examined to determine
to determine the
determine the
the
weak interlayer
weak
weak interlayer bonding.
interlayer bonding. As
bonding. As the
As the layer
the layer thickness
layer thickness increases,
thickness increases, the
increases, the accuracy
the accuracy
accuracy of of the
of the overall
the overall finished sample
overall finished
finished sample
sample
geometry decreases
geometry
geometry decreases and
decreases and the
and the outline
the outline more
outline more readily
more readily displays
readily displays the
displays the staircase
the staircase phenomenon.
staircase phenomenon.
phenomenon.
3.2. Comparison
3.2.
3.2. Comparison of
Comparison of ABS
of ABS and
ABS and PEEK
and PEEK Tensile
PEEK Tensile Strengths
Tensile Strengths
Strengths
To evaluate
To evaluate the
evaluate the performance
the performance of
performance of printed
printed PEEK
PEEK samples,
samples, we
we built
built samples
samples fromfrom PEEK
PEEK and
and ABS
ABS
using optimal
using optimal parameters.
parameters. Figure
Figure
Figure 33 shows
shows ABS
ABS and
and PEEK
PEEK samples
samples after
after the
the tensile
the tensile test.
tensile test. Engineering
test. Engineering
stress-strain curves
stress-strain curves for
for PEEK
PEEK and
and ABS
ABS samples
samples are
are shown
shown in
shown in Figure
in Figure 4.
Figure 4.
4.
Figure 3.3.
Figure
Figure 3. Fractured
Fractured tensile
Fractured tensilesamples.
tensile samples. (a)
samples. (a)acrylonitrile
(a) acrylonitrilebutadiene
acrylonitrile butadiene
butadiene styrene
styrene (ABS);
(ABS);
styrene (b)
(ABS);
(b) polyether-ether-ketone
polyether-ether-ketone
polyether-ether-ketone
(b) (PEEK).
(PEEK).
(PEEK).
Figure
Figure 4. Tensile stress-strain
4. Tensile
Tensile stress-strain curves
curves of
of acrylonitrile
acrylonitrile butadiene
butadiene styrene
styrene (ABS)
(ABS) and
and
Figure 4. stress-strain curves of acrylonitrile butadiene styrene (ABS) and
polyether-ether-ketone (PEEK).
polyether-ether-ketone (PEEK).
(PEEK).
polyether-ether-ketone
The ABS
The
The ABS curve
ABS curve includes
curve includes regions
includes regions of
regions of elastic
of elastic and
elastic and plastic
and plastic deformation,
plastic deformation, accompanied
deformation, accompanied by
accompanied by necking
by necking
necking
deformation. The
deformation.
deformation. The stress-strain
The stress-strain behavior
stress-strain behavior under tensile
behavior under
under tensile stress
tensile stress was
stress was initially
was initially nonlinear.
initially nonlinear. After
nonlinear. After the
After the sample
the sample
sample
Materials 2015, 8 5840
Materials 2015, 8 3889
reached peak stress, the resisting stress was almost constant with the increase in strain through shape. It
reached peak stress, the resisting stress was almost constant with the increase in strain through shape.
can be concluded that the fracture of ABS occurs mainly via damage to the raster. As the tensile stress
It can be concluded that the fracture of ABS occurs mainly via damage to the raster. As the tensile
increases, the failure will begin at the weakest raster and next weakest raster will break, in sequence,
stress increases, the failure will begin at the weakest raster and next weakest raster will break,
until total failure of the sample. When the stress reaches a certain constant value, a long propagation
in sequence, until total failure of the sample. When the stress reaches a certain constant value, a long
process
propagationoccurs in theoccurs
process neck.inCraze is the
the neck. mainis plastic
Craze the main deformation mechanism
plastic deformation of ABS, of
mechanism with
ABS,a great
with
number of crazes appearing perpendicular to the direction of the tensile loading.
a great number of crazes appearing perpendicular to the direction of the tensile loading. Crazes initiate, Crazes initiate, widen,
then
widen,suffer
thenbreakdown of the raster
suffer breakdown as tension
of the raster asincreases. If crazes extend
tension increases. to both
If crazes endstoofboth
extend the sample,
ends of the
the
sample fails with insignificant necking deformation, because molecular chains
sample, the sample fails with insignificant necking deformation, because molecular chains initially in initially in an unoriented
state transformstate
an unoriented to a transform
more highly to aoriented
more highlystate of necking.
oriented stateThe transformation
of necking. process causesprocess
The transformation strain
hardening,
causes strain and ensures the
hardening, anduniform
ensures expansion
the uniformofexpansion
crazes extending
of crazestoextending
both ends, to which
both ends,is similar
which tois
metal deformation hardening caused by uniform deformation.
similar to metal deformation hardening caused by uniform deformation.
The
The PEEK
PEEK curvecurve clearly
clearly differs
differs from
from the the ABS
ABS curve.
curve. As Asthe theload
loadincreased,
increased,PEEK PEEKfirstfirstyielded
yieldedatata
amaximum
maximumstress, stress,then
thennecking
neckingdeformation
deformationappeared
appearedatat the the tensile
tensile fracture
fracture surface
surface andand thethe samples
samples
broke after reaching the maximum stress, when the strain reached
broke after reaching the maximum stress, when the strain reached 87%. In PEEK samples, there 87%. In PEEK samples, there waswasno
obvious
no obvious necking deformation
necking deformationat the tensile
at the fracture
tensile surface,
fracture and and
surface, no obvious
no obviousneckneck
propagation
propagation untiluntil
the
fracture of samples
the fracture of samplesafterafter
yielding.
yielding.
Figure
Figure 5 shows the average tensile
5 shows the average tensile property
property values
values forfor both
both ABSABS and and PEEK.
PEEK. The The elastic
elastic limit
limit from
from
five tensile experiments with PEEK was 50.8 MPa; the tensile strength
five tensile experiments with PEEK was 50.8 MPa; the tensile strength of PEEK was 56.6 MPa, while of PEEK was 56.6 MPa, while
the
the elastic
elastic limit
limit ofof ABS
ABS was was 22.9
22.9 MPa,
MPa, and and the
the tensile
tensile strength
strength of of ABS
ABS waswas 27.1
27.1 MPa.
MPa. TheThe values
values ofof
these
these properties
propertiesfor forPEEK
PEEKwere were 122%
122% andand108%108% higher thanthan
higher for ABS. As shown
for ABS. in the in
As shown figure, the tensile
the figure, the
properties of 3D-printed ABS samples were lower than injection-molded
tensile properties of 3D-printed ABS samples were lower than injection-molded ABS by 26.2% for the ABS by 26.2% for the elastic
elasticand
limit limit
26.8%and for
26.8% for thestrength.
the tensile tensile strength.
Likewise, Likewise,
the tensile theproperties
tensile properties of 3D-printed
of 3D-printed PEEK samplesPEEK
samples
were lower were
thanlower than injection-molded
injection-molded PEEK by 29.4% PEEKforbythe29.4% elasticforlimittheand
elastic
43.4% limit andtensile
for the 43.4%strength.
for the
tensile strength.
However, the lowerHowever,
strengththeoflower strength
3D-printed of 3D-printed
samples compared samples compared with injection-molded
with injection-molded samples can be
samplesattributed
mainly can be to mainly attributed
the gaps betweentofilaments
the gapsand between filaments
the extensive poresand the filaments,
within extensive especially
pores within for
filaments,
PEEK especially
samples because forofPEEK samples
the poor because
printing qualityof obtained.
the poor printing quality obtained.
Figure
Figure 66 shows
shows scanning
scanning electron
electron microscopy
microscopy (SEM)
(SEM) images
images of of fracture
fracture cross-sections
cross-sections of of PEEK
PEEK and and
ABS along the longitudinal direction. These images of the fracture surface show
ABS along the longitudinal direction. These images of the fracture surface show that failure was that failure was caused
by differing
caused reasons. Although
by differing reasons. ABS individual
Although ABSrasters had melted
individual rasterstogether, we cantogether,
had melted still distinguish
we canevery still
raster in the images, and the fracture of ABS was mainly caused by damage to
distinguish every raster in the images, and the fracture of ABS was mainly caused by damage to the the rasters pulling and
rupturing. As the
rasters pulling andload force increased,
rupturing. the force
As the load force per unit areathe
increased, would
forcereach the filaments
per unit area would tensile
reachlimit.
the
In the printed samples the fracture would begin approximately at the weakest filament,
filaments tensile limit. In the printed samples the fracture would begin approximately at the weakest and the fracture
would
filament,propagate
and theuntil the samples
fracture would failed. The result
propagate is that
until the the stress
samples continues
failed. to increase
The result is thatandthe
thestress
next
weakest
continuesraster will fail.and
to increase Bytheobserving the failure
next weakest rastersurfaces
will fail.ofBy
PEEK samples,
observing thewe can see
failure that there
surfaces were
of PEEK
no obvious
samples, werasters
can seeand
that thethere
samples
wereappeared
no obviousto have melted
rasters and theintosamples
a block.appeared
This was to most
have likely
meltedcaused
into a
by a combination of the high extruder temperature and filaments that created significant
block. This was most likely caused by a combination of the high extruder temperature and filaments thermal bonding
between bothsignificant
that created raster andthermal
layers, causing
bondinggreater
between fusion.
both raster and layers, causing greater fusion.
Properties
3.3. Comparison of ABS and PEEK Compressive Properties
deformation appears
deformation appearstoto
appears toresult
resultfrom
result from
from extensive
extensive
extensive pores
pores
pores becoming
becoming
becoming squeezed
squeezed
squeezed out.
out. out. Ifcould
If weIf we could
we could reduce
reducereduce the
the
the pores
pores within
pores
withinwithin the printed
the
the printedprinted part,
part,
part, the the compressive
the compressive
compressive strength
strengthstrength and printing
and
and printing printing quality
quality
quality of of 3D-printed
of
3D-printed3D-printed PEEK
PEEK
PEEK parts parts
parts
could be
could
could be substantially
be substantially
substantially improved.
improved.improved.
7. Fractured
Figure 7.
Figure 7. Fractured
Fractured compressive
compressive samples. (a)
(a) acrylonitrile
compressive samples. (a)
acrylonitrile butadiene
butadiene styrene (ABS);
acrylonitrile butadiene styrene (ABS);
polyether-ether-ketone
(b) polyether-ether-ketone (PEEK).
(PEEK).
(b) polyether-ether-ketone (PEEK).
3.4. Comparison
3.4. Comparison of
of ABS
ABS and
and PEEK
PEEK Bending
Bending Properties
Properties
Figure
Figure 10
10 shows
shows ABS
ABS andand PEEK
PEEK samples
samples after
after three-point
three-point bending
bending tests.
tests. Figure
Figure 11
11 shows
shows bending
bending
engineering
engineering stress-strain
stress-straincurves
curvesforfor
ABSABSand and
PEEK samples.
PEEK According
samples. to the GB/T9341-2008
According bending
to the GB/T9341-2008
standard,standard,
bending the bending
the strength
bending is set as the
strength value
is set thatvalue
as the causesthat3.5% deformation.
causes The bending
3.5% deformation. The strength
bending
strength and bending modulus of five experiments are shown in Figure 12. The bending strengthwas
and bending modulus of five experiments are shown in Figure 12. The bending strength of PEEK of
PEEK
56.2 was 15%
MPa, 56.2 higher
MPa, 15%than higher
that ofthan
ABSthat of ABS
(48.6 MPa).(48.6TheMPa).
bendingThemodulus
bending ofmodulus
PEEK of wasPEEK was
1.6 GPa,
1.6 GPa,
which waswhich
very was
closevery closeoftoABS.
to that that ofThe
ABS.
mainThereason
main for
reason
the for theflexural
poor poor flexural
propertyproperty
is the is the
weak
interlayer
weak bonding.
interlayer The 3D-printed
bonding. ABS samples
The 3D-printed had bending
ABS samples strengthstrength
had bending and bending modulus modulus
and bending reduced
by up toby
reduced 8.2%up and 20.8%,
to 8.2% andrespectively, compared compared
20.8%, respectively, with thosewith of injection-molded ABS. The ABS.
those of injection-molded weak
The weakbonding
interlayer interlayer bonding
greatly greatly
influenced influenced
3D-printed PEEK3D-printed PEEK sample
sample properties, properties,
because because
the bending the
strength
bending
and strength
bending and bending
modulus modulus
were reduced were
by up reducedand
to 65.5% by58.9%,
up to 65.5% and 58.9%, respectively.
respectively.
Figure 10.
Figure Fractured bending
10. Fractured bending samples.
samples. (a)
(a) acrylonitrile
acrylonitrile butadiene
butadiene styrene
styrene (ABS);
(ABS);
(b) polyether-ether-ketone (PEEK).
(b) polyether-ether-ketone (PEEK).
Materials 2015, 8 5844
Materials 2015, 8 3893
by 108%, 114% and 115%, respectively, while little significant difference was found between the
compressive and flexural modulus of PEEK and ABS. Experimental studies and comparative analyses
were carried out to study the factors affecting PEEK 3D print forming quality, in the hope of providing
reference conditions under which to print PEEK. However, we recognize that there is much work left to
do in this area. Further research is needed to reduce pore formation during the printing process and to
improve interlayer bonding. PEEK has favorable properties, including excellent mechanical properties
in both static and dynamic tests and high chemical resistance [21,22]. It is believed that PEEK may be a
significant and promising material for industrial applications of 3D-printed components.
Acknowledgments
This research is supported by National Natural Science Foundation of China (No. 51205163),
Specialized Research Fund for the Doctoral Program of Higher Education of China SRFDP
(No. 20120061120030), Young Research Fund of Jilin Province Science and Technology Development
Plan (No. 20140520124JH) and Young Teachers and Students to Interdisciplinary Cultivating Project of
Jilin University (No. JCKY-QKJC28).
Author Contributions
Wenzheng Wu designed the experiment and wrote the final manuscript. Peng Geng Guiwei Li and
Di Zhao wrote the first draft and prepared the experiment. Haibo Zhang carried out the experimental
study. Ji Zhao supervised the research, design of the study and carried out the conception. All authors
contributed to the analysis for results and conclusions and revised the paper.
Conflicts of Interest
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