polymers

Article
Evaluation of the Mechanical and Tribological Behavior of
Polyether Ether Ketone Fiber-Reinforced Resin-Based Friction
Materials Fabricated by Wet Granulation
Lekai Li 1,2,3 , Zichao Ma 4 , Guoqin Liu 1,2,3 , Wei Song 5 , Lili Ren 1 , Shengwang Yuan 1,2,3 , Xiao Yang 1,3 ,
Qifeng Zhang 1,3 and Yunhai Ma 1,2,3, *

1 Key Laboratory of Bionic Engineering (Ministry of Education), College of Biological and Agricultural
Engineering, Jilin University, Changchun 130022, China; [email protected] (L.L.);
[email protected] (G.L.); [email protected] (L.R.); [email protected] (S.Y.);
[email protected] (X.Y.)
2 Institute of Structured and Architected Materials, Liaoning Academy of Materials, Shenyang 110167, China
3 Weihai Institute for Bionics, Jilin University, Weihai 264200, China
4 Department of Mechanical Engineering, The Pennsylvania State University, State College, PA 16801, USA;
[email protected]
5 The College of Engineering and Technology, Jilin Agricultural University, Changchun 130022, China;
[email protected]
* Correspondence: [email protected]

Abstract: Resin-based friction materials (RBFMs) strengthened by polyether ether ketone (PEEK)
fiber were designed and prepared in this study. Specimens incorporating PEEK fiber of 2–8 wt.% were
fabricated based on wet granulation, and then the effects of the PEEK fiber content on the mechanical
and tribological properties of RBFMs were systematically investigated. The results showed that PEEK
fiber can sense the braking temperature and then effectively regulate the comprehensive properties
of RBFMs. The specimen incorporating 6 wt.% PEEK fiber obtained the optimal comprehensive
performance with a stable friction coefficient (COF), excellent fade resistance and recovery properties,
Citation: Li, L.; Ma, Z.; Liu, G.; Song, and better wear resistance. The worn surface was inspected using a scanning electron microscope.
W.; Ren, L.; Yuan, S.; Yang, X.; Zhang, After the friction–wear test, the specimen with 6 wt.% PEEK fiber presented a number of primary
Q.; Ma, Y. Evaluation of the
and secondary plateaus and a reduced number of pits with wear debris on the worn surface. The
Mechanical and Tribological Behavior
study indicated that PEEK fiber could not only enhance the mechanical and tribological properties
of Polyether Ether Ketone
of RBFMs at low temperatures because of their high strength and self-lubrication but also adhere
Fiber-Reinforced Resin-Based Friction
to wear debris to reduce abrasive wear at high temperatures; furthermore, the adhered wear debris
Materials Fabricated by Wet
Granulation. Polymers 2023, 15, 4732.
could form a secondary plateau under normal pressure, which could alleviate abrasion.
https://doi.org/10.3390/
polym15244732 Keywords: resin-based friction materials; PEEK fiber; wet granulation; tribological properties

Academic Editor: Ankit Gupta

Received: 4 November 2023

Revised: 8 December 2023 1. Introduction
Accepted: 12 December 2023 With the development of technology and the economy, means of transportation such
Published: 18 December 2023 as automobiles and trains are playing a more and more important role in human society,
and they have continually increasing requirements in terms of speed, safety and comfort [1].
As an important part in brake systems, resin-based friction materials (RBFMs) are the last
Copyright: © 2023 by the authors.
line of defense for safe operation; their stability and reliability are directly related to the
Licensee MDPI, Basel, Switzerland.
safety of passengers [2,3]. At present, friction materials applied to brake systems can be
This article is an open access article divided into four categories: ceramic-based friction materials, resin-based friction materials,
distributed under the terms and powder metallurgy friction materials, and C/C composite materials [4–6]. Among them,
conditions of the Creative Commons RBFMs are widely used because of their simple preparation and low cost [4].
Attribution (CC BY) license (https:// RBFMs are usually strengthened by reinforced fibers because of their high strength
creativecommons.org/licenses/by/ and high modulus [7,8]. Generally speaking, from the macro-perspective, reinforced fibers
4.0/). have a high modulus, high strength, and good thermal and tribological stability, which

Polymers 2023, 15, 4732. https://doi.org/10.3390/polym15244732 https://www.mdpi.com/journal/polymers

Polymers 2023, 15, x FOR PEER REVIEW 2 of 15

Polymers 2023, 15, 4732 RBFMs are usually strengthened by reinforced fibers because of their high strength 2 of 14
and high modulus [7,8]. Generally speaking, from the macro-perspective, reinforced fibers
have a high modulus, high strength, and good thermal and tribological stability, which
used to
can be used to enhance
enhance strength,
strength, fade
fade resistance
resistance (the
(the resistance
resistance of of the
the friction
friction coefficient
coefficient
(COF) to
(COF) tohigh-temperature
high-temperaturereduction),
reduction),and and wear
wear resistance
resistance [9].[9]. From
From thethe micro-perspec-
micro-perspective,
tive, reinforced
reinforced fibers fibers
play aplay a positive
positive role in role in consolidating
consolidating wear and
wear debris, debris,
theyandare they are the
the primary
plateau,
primary which
plateau,canwhich
produce
cannucleation of wear debris,
produce nucleation of wearthus promoting
debris, the formation
thus promoting the of
for-a
secondary
mation of aplateau [10–12].
secondary Commonly
plateau [10–12].used reinforced
Commonly usedfibers includefibers
reinforced metal include
fiber (suchmetalas
steel
fiber fiber
(suchand copper
as steel fiber,
fiber and etc.),
copperglass fiber,
fiber, carbon
etc.), glass fiber,
fiber, ceramic fiber,ceramic
carbon fiber, and organicfiber,fiber
and
(including
organic fiber synthetic and natural
(including fibers,
synthetic andsuch as cotton
natural fibers,fiber
suchandas corn stalk
cotton fiber,
fiber andetc.)
corn [13,14].
stalk
The
fiber,classification and classification
etc.) [13,14]. The characteristics andofcharacteristics
reinforced fibers used in RBFMs
of reinforced are shown
fibers used in RBFMs in
Figure
are shown1. in Figure 1.

Figure 1.
Figure 1. Classification
Classification and
and characteristics
characteristics of
of reinforced
reinforced fibers
fibers used
used in
in RBFMs.
RBFMs.

Reinforced fibers
fibers play
playan animportant
importantrole roleinin RBFMs.
RBFMs. Carbon
Carbon fiberfiber canonly
can not not only
enhanceen-
hance the mechanical
the mechanical strength strength
of RBFMs of RBFMs
but alsobut also reduce
reduce abrasion abrasion
becausebecause
of their of their self-
self-lubrica-
lubrication, high temperature
tion, high temperature resistance, resistance,
and other andexcellent
other excellent properties
properties (Farhad(Farhad Ahmadi-
Ahmadijokani et
jokani et al.) [12,15,16].
al.) [12,15,16]. Metal fibersMetalhavefibers
highhave high strength
strength and highand heathigh heat conductivity,
conductivity, which can which
im-
can
proveimprove
the heat the heat conductivity
conductivity of friction
of friction materials, materials, thus preventing
thus preventing COF heat COF heat during
fading fading
during braking (Sung Bin Park, H. Jang et al.) [17,18]; however, because
braking (Sung Bin Park, H. Jang et al.) [17,18]; however, because of the environmental of the environmental
pollution
pollutioncaused
causedby bycopper
copper fiber,
fiber,they have
they limited
have incorporation
limited in RBFMs
incorporation in RBFMs(Jian (Jian
Xian, Xian,
Yang
et al.) [19,20]. Natural fibers, which are renewable and non-polluting,
Yang et al.) [19,20]. Natural fibers, which are renewable and non-polluting, have recently have recently become
abecome
research hotspot within
a research hotspotthewithinfield the
of reinforced fibers (Yunhai
field of reinforced Ma [3], Yucheng
fibers (Yunhai Liu [21]
Ma [3], Yucheng
et
Liual.). Although
[21] these fibers
et al.). Although these canfibers
improve tribological
can improve properties
tribological to a certain
properties to aextent,
certainthey
ex-
cannot adapt themselves to different braking conditions, and their
tent, they cannot adapt themselves to different braking conditions, and their tribological tribological properties
are still poor
properties areatstill
higher
poorbraking
at higher temperatures [22,23].
braking temperatures [22,23].
Polyether
Polyether ether ketone (PEEK) fiber can reduce abrasion
ether ketone (PEEK) fiber can reduce abrasion and
and improve
improve the the mechanical
mechanical
strength of RBFMs because of their high strength
strength of RBFMs because of their high strength and self-lubricationand self-lubrication [24,25]. Furthermore,
[24,25]. Further-
PEEK ◦
more, will
PEEK stay
willmolten at highattemperatures
stay molten high temperatures (more (more
than 343thanC)343and
℃)can andadhere to wear
can adhere to
debris to decrease abrasion [26–28]. The adherent wear debris will
wear debris to decrease abrasion [26–28]. The adherent wear debris will form a secondary form a secondary plateau
under normal pressure, thus protecting RBFMs and enhancing wear resistance [25]. The
plateau under normal pressure, thus protecting RBFMs and enhancing wear resistance
characteristics of PEEK fiber provide a good reference for the design of RBFMs. However,
[25]. The characteristics of PEEK fiber provide a good reference for the design of RBFMs.
the application of PEEK fiber in RBFMs is rarely reported.
However, the application of PEEK fiber in RBFMs is rarely reported.
Aiming at enhancing the comprehensive properties of RBFMs in different braking
Aiming at enhancing the comprehensive properties of RBFMs in different braking
conditions, PEEK fiber was incorporated into RBFMs in this study, which responded to
conditions, PEEK fiber was incorporated into RBFMs in this study, which responded to
the external stimulus with a specific manner and exhibited some desirable behaviors.
Firstly, PEEK fiber can enhance the impact strength of RBFMs, which was important for
its comprehensive performance. Secondly, molten PEEK can adhere to wear debris on
the friction surface at high temperatures, which can alleviate abrasive wear; at the same
Polymers 2023, 15, 4732 3 of 14

time, the adhered wear debris can form a secondary plateau under normal pressure to
protect RBFMs. Thirdly, the self-lubrication property of PEEK fiber can reduce abrasion
and enhance the service life.

2. Materials and Methods

2.1. Raw Materials
The raw materials in this study mainly included PEEK fiber, sepiolite fiber, compound
mineral fibers, phenolic powder, graphite, petroleum coke, aluminum oxide, friction dust
(cashew nut shell oil), calcium carbonate, vermiculite powder, barium sulfate, and zinc
stearate. The content of barium sulfate decreased step by step with increasing PEEK fiber
content because barium sulfate has a smaller effect on the tribological properties of RBFMs.
The content of raw materials and their information are shown in Tables 1 and 2, respectively.

Table 1. Composition of the prepared specimens.

Raw Materials (by wt.%) Specimens

and Size (by Mesh) PFS-0 PFS-2 PFS-4 PFS-6 PFS-8
PEEK fiber (0.1 mm× 3 mm) 0 2.00 4.00 6.00 8.00
Sepiolite fiber (0.15 mm × 2.5 mm) 5.00 5.00 5.00 5.00 5.00
Compound mineral fibers (0.2 mm × 3 mm) 20.00 20.00 20.00 20.00 20.00
Phenolic powder (200) 9.00 9.00 9.00 9.00 9.00
Graphite (100) 8.00 8.00 8.00 8.00 8.00
Petroleum coke (400) 7.00 7.00 7.00 7.00 7.00
Aluminum oxide (325) 6.00 6.00 6.00 6.00 6.00
Friction dust (cashew nut shell oil, 100) 2.00 2.00 2.00 2.00 2.00
Calcium carbonate (1250) 13.00 13.00 13.00 13.00 13.00
Vermiculite powder (30) 5.00 5.00 5.00 5.00 5.00
Barium sulfate (325) 24.00 22.00 20.00 18.00 16.00
Zinc stearate (200) 1.00 1.00 1.00 1.00 1.00

Table 2. The information of raw materials.

Raw Materials Information

Raw Materials
Purity Supply Function
Changzhou Chuangying Reinforce mechanical
PEEK fiber New Material Technology strength, adhering wear
Co., LTD, Changzhou, China debris on worn surface
Lingshou Jiasuo Building
Reinforce mechanical
Sepiolite fiber 99% Materials Processing Co.,
strength
LTD, Shijiazhuang, China
SiO2 : 40–43%; Al2 O3 :16–18%; CaO: Shijiazhuang Mayue
Compound mineral Reinforce mechanical
14–16%; MgO: 5–7%; Fe2 O3 : 3–5%; C: Building Materials Co., LTD,
fibers strength
4–6% Shijiazhuang, China
Henan Borun Casting Adhere to the other
Phenolic powder Material Co., LTD, Gongyi, reinforcement components
China
Henan Borun Casting
Form friction film to enhance
Graphite 99.5% Material Co., LTD, Gongyi,
tribological properties
China
Shijiazhuang Yuxin Building
Reduce COF and specific
Petroleum coke 85% Materials Co., LTD,
wear rate
Shijiazhuang, China
Henan Borun Casting Reduce adhesive wear,
Aluminum oxide 99.9% Material Co., LTD, Gongyi, enhance COF and wear
China resistance
 Shijiazhuang Yuxin Building
Reduce COF and sp
Petroleum coke 85% Materials Co., LTD, Shijia-
wear rate
zhuang, China
Polymers 2023, 15, 4732
Reduce adhesive we
Aluminum ox- Henan Borun Casting Mate- 4 of 14
99.9% hance COF and we
ide rial Co., LTD, Gongyi, China
sistance
Table 2. Cont.
Friction dust
Zhejiang Jiamin Plastic Co., Improve braking stab
(cashew nut Raw Materials Information
Raw Materials LTD, Jiaxing, China reduce braking n
shell oil) Purity Supply Function
Friction dust (cashew Shandong
Zhejiang Yusuo
Jiamin Plastic Co.,Chemical
Improve braking stability
Calciumnutcar-
shell oil) LTD, Jiaxing, China and reduce braking noisy
99% Technology Co., LTD, Linyi, Filler in RBFM
bonate
Shandong Yusuo China
Chemical
Calcium carbonate 99% Technology Co., LTD, Linyi, Filler in RBFMs
Vermiculite Lingshou Xuyang Mining Co., Reduce braking noi
China
powder LTD,Xuyang
Lingshou Shijiazhuang,
Mining China density of RBFM
Reduce braking noise and
Vermiculite powder Co., LTD, Shijiazhuang,
Shandong Yusuo Chemical density of RBFMs
China
Barium sulfate ≥98% Technology Co., LTD, Linyi,
Shandong Yusuo Chemical
Reduce braking n
Barium sulfate ≥98% China
Technology Co., LTD, Linyi, Reduce braking noise
China
Zinc content: 11.01%; Free acid content: Wuxi Yatai Joint Chemical
Zinc stearate Zinc content: 11.01%; Free acid content: Wuxi Yatai Joint Chemical Lubrication
Zinc stearate 0.47%; Moisture content: 0.37%
0.47%; Moisture content: 0.37%
Co., LTD, Wuxi, China Lubrication
Co., LTD, Wuxi, China

2.2.Fabrication
2.2. Fabrication of Specimen
of Specimen
The
The main
main fabrication
fabrication steps ofsteps
RBFMs ofwere
RBFMs were step
step mixing, mixing, wet
wet granulation, hot granulation,
pressing, h
and
ing,heat
and treatment [21,25]. The
heat treatment fabrication
[21,25]. Theprocess is shown
fabrication in Figure
process is 2.
shown in Figure 2.

Figure
Figure 2. Fabrication
2. Fabrication process
process of RBFMs.
of RBFMs.

Firstly, the raw materials were mixed using an electrical blender (JF801S, Wangda,
Firstly,
Changchun, the Reinforced
China). raw materials were
fibers such as mixed
sepioliteusing an electrical
fiber, compound mineralblender (JF801S, W
fibers, and
Changchun,
PEEK fiber wereChina).
mixed for Reinforced fibers such
3–5 min to improve as sepiolite
dispersion. Then, allfiber,
other compound
composition miner
andthrown
were PEEKinto fiber were mixed
a compact for 3–5
rake blender minWangda,
(JF810, to improve dispersion.
Changchun, China) Then, all other c
for mixing,
the mixing time was 8–10 min.
tion were thrown into a compact rake blender (JF810, Wangda, Changchun, Ch
Secondly, prefabricated particles were prepared by wet granulation using a laboratory
mixing, the mixing time was 8–10 min.
tumbling granulator (JF805R, Wangda, Changchun, China). The wet granulation process is
Secondly,
presented in Figure prefabricated particles
3. The bridging liquid were prepared
was absolute byand
ethyl alcohol, wetthegranulation
total quantity using a
tory tumbling granulator (JF805R, Wangda, Changchun, China). The wet
was about 40 wt.% of the mixture. After wet granulation, the prefabricated particles weregranula
dried
cess using a heat-treated
is presented case (JF980S,
in Figure 3. TheWangda,
bridging Changchun,
liquid was China).
absolute ethyl alcohol, and
quantity was about 40 wt.% of the mixture. After wet granulation, the prefabrica
ticles were dried using a heat-treated case (JF980S, Wangda, Changchun, China).
 Polymers2023,
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Polymers 2023,15,
2023, 15,4732
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FOR PEER
PEER REVIEW
REVIEW 555 of
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14

Figure3.3.
Figure
Figure 3.The
Theprocess
The processof
process ofwet
of wetgranulation.
wet granulation.
granulation.

Thirdly,the
Thirdly,
Thirdly, theprefabricated
the prefabricatedparticles
prefabricated particleswere
particles werepressed
were pressedfor
pressed for10
for 10min
10 minatat
min 160◦ C
at160
160 ℃℃under
under45
under 45MPa
45 MPa
MPa
for
for hot
hot pressing
pressing [25];
[25]; the
the pressing
pressing device
device was
was a
a hot
hot compression
compression machine
machine
for hot pressing [25]; the pressing device was a hot compression machine (JFY50, Wangda,(JFY50,
(JFY50, Wangda,
Wangda,
Changchun,China).
Changchun,
Changchun, China).During
China). Duringhot
During hotpressing,
hot pressing,three
pressing, threeintermittent
three intermittent‘breathings’
intermittent ‘breathings’were
‘breathings’ wereconducted
were conducted
conducted
torelease
to
to releasevolatiles.
release volatiles.After
volatiles. Afterhot
After hotpressing,
hot pressing,the
pressing, thespecimens
the specimenswere
specimens wereheat
were heattreated
heat treatedby
treated byaaaheat-treated
by heat-treated
heat-treated
case
case(JF980S,
(JF980S,Wangda,
Wangda, Changchun,
Changchun, China)
China)to remove
to remove the remaining
the remaining stress;
case (JF980S, Wangda, Changchun, China) to remove the remaining stress; the tempera- the
stress; temperature
the tempera-
evolution
ture during
evolution heat
during treatment
heat is given
treatment is in Figure
given in
ture evolution during heat treatment is given in Figure 4. 4.
Figure 4.

Figure 4.Heat-treatment
Figure4.4.
Figure Heat-treatmenttemperature
Heat-treatment temperatureofof
temperature ofspecimens.
specimens.
specimens.
2.3. Testing Methods and Equipment
2.3. Testing
2.3. Testing Methods
Methods and
and Equipment
Equipment
Thermogravimetric analysis (TGA) was conducted using a TA thermogravimetric
Thermogravimetric analysis
Thermogravimetric analysis (TGA)
(TGA) was
was conducted using
using aa TA
TA thermogravimetric
thermogravimetric an- an-
analyzer (TGA55, TA, Delaware, USA) underconducted
nitrogen, the temperature range from 30 to
alyzer
alyzer (TGA55,
(TGA55, TA, Delaware,
TA, Delaware, USA) under nitrogen, the temperature range from 30 to 400
400 ◦ C and the heating rate of 5USA) under
◦ C/min. Thenitrogen, thespecimens
density of temperature wasrange
testedfrom 30 on
based to 400
an
°C and
°C and the
the heating
heating rate
rate of
of 55 °C/min.
°C/min. TheThe density
density of
of specimens
specimens was was tested
tested based
based onon an
an
Archimedes Drainage Principle, the hardness of samples was tested by a rockwell hardness
Archimedes
Archimedes Drainage Principle,
Drainage(HRSS-150, the
Principle, the hardness of samples
hardnessChina),
of samples was tested
wasimpact by a
tested strength rockwell
by a rockwell hard-
hard-
measuring instrument Hangzhou, and the was tested
ness measuring
ness measuring instrument
instrument (HRSS-150,
(HRSS-150, Hangzhou,
Hangzhou, China),
China), and
and thethe impact
impact strength
strength waswas
by an impact tester (XJ-40A, Jinan, Shandong, China). Impact strength was tested according
tested by
tested by an
an impact
impact tester
tester (XJ-40A,
(XJ-40A, Jinan,
Jinan, Shandong,
Shandong, China).
China). Impact
Impact strength
strength waswas tested
tested
to GB/T 33835-2017; the specimens were cut as 55 mm × 6 mm × 4 mm; the maximum
according to
according to GB/T 33835-2017;
33835-2017; the specimens
specimens were cut cut as
as 55
55 mmmm ×× 66 mmmm × 4 mm; mm; the
impact energy,GB/T
swing angle, andthe impact speed wereof the pendulum were 0.981 ×J, 4150 the
◦ , and
maximum
maximum impact energy,
impact energy, swing angle,
swing angle, and impact
and of
impact speed of
speededge the
of the pendulum were 0.981 J,
2.9 m/s, respectively. Furthermore, the angle the cutting of pendulum
the striker waswere750.981
◦ andJ,
150°,
150°,
the
and 2.9
and 2.9
filleted
m/s, respectively.
m/s,ofrespectively.
corner
Furthermore,
Furthermore,
the cutting edge
the angle
the Each
was 0.8 mm.
of the
anglesample cutting
of the cutting
was tested
edge
edge of the
oftimes,
five
striker
the striker
and
the final results were the average value of the performed 5 tests.
Polymers 2023, 15, x FOR PEER REVIEW 6 of 15

Polymers 2023, 15, 4732 6 of 14

was 75° and the filleted corner of the cutting edge was 0.8 mm. Each sample was tested
five times, and the final results were the average value of the performed 5 tests.
The
The tribological performance of
tribological performance of specimens
specimens was was evaluated
evaluated by by aa constant-speed
constant-speed tester tester
(JF150F-II, Wangda, Changchun, China, shown in
(JF150F-II, Wangda, Changchun, China, shown in Figure 5) according toFigure 5) according to GB/T
GB/T 5763-2008.
5763-2008.
The materials
The materials of the brake
of the brake disc
disc were
were graygray cast iron whose
cast iron whose main main component
component was was pearlite;
pearlite;
the hardness of the brake disc was between 180 and 220 HB; the
the hardness of the brake disc was between 180 and 220 HB; the diameter, thickness, and diameter, thickness, and
roughness
roughness of of the
the counterpart
counterpart was was 373
373 mm,
mm, 20 20 mm,
mm, andand 3.23.2 µm,
µm, respectively.
respectively. The The specimen
specimen
size
size of
of RBFMs
RBFMs was was25 25mmmm××2525mm mm × 6×mm;6 mm; thethe
distance
distancefrom the the
from specimen
specimen center to the
center to
brake disc center was 0.15 m. During a friction-wear test, the rotation
the brake disc center was 0.15 m. During a friction-wear test, the rotation speed of the speed of the brake
disc
brake and loading
disc pressure
and loading were constant
pressure at 480 r/min
were constant at 480 and 0.98 and
r/min MPa,0.98respectively. The fric-
MPa, respectively.
The friction-wear test can be divided into two stages, the first stage was a fade testthe
tion-wear test can be divided into two stages, the first stage was a fade test and andtem-
the
peratures
temperatures of the brake
of the brakedisc were
disc weresetsetasas100100℃,C,150
◦ 150℃,C,200
◦ 200℃,C,250
◦ 250℃, ◦ 300℃Cand
C,300 ◦ and 350350 ℃,
◦ C,
respectively (the temperature
temperature of of the brake disc was regulated mainly by cooling water and
a thermoelectric couple inside the brake disc. The cooling water and thermoelectric were
controlled computer). Before
controlled by the computer). Before the
the formal
formal test,
test, specimens
specimens were were run
run below
below 100100 ◦℃ C until
the contact area reached more than 95%, and then the initial thickness
contact area reached more than 95%, and then the initial thickness of the specimen of the specimen was
measured
was measuredwithwith
a spiral micrometer.
a spiral micrometer. EachEachsamplesamplewas was
measured
measuredat 5 atdifferent points
5 different (in-
points
cluding 4 corner
(including 4 cornerpoints
pointsandand
1 central
1 centralpoint) andand
point) theythey
were entered
were intointo
entered the the
computer
computer be-
before
fore thethe formal
formal testtest
waswas carried
carried out.
out. During
During thethefade fade
test,test,
the the brake
brake discdisc would
would rotate
rotate for
for 5000
5000 r and
r and would
would automatically
automatically stop
stop atateach
eachtemperature;
temperature;then, then,thethe specimen
specimen thickness
was measured again and input into the computer to automatically calculate COF and SWR
according to formulas (1) and (2). The second stage was a recovery test. In this stage, the
◦ C, 200 ◦ C, 150 ◦ C and 100 ◦ C successively. At
temperatures was reduced reduced from
from 300
300 toto250250 ℃, 200 ℃, 150 ℃ 100 ℃ successively.
each temperature,
temperature,the thebrake discdisc
brake rotated
rotated15001500
r untilr the
untilfriction disc automatically
the friction stopped.
disc automatically
After continuous
stopped. rotation ofrotation
After continuous 7500 r, the computer
of 7500 r, thewould
computeroutput COF output
would at each COFtemperature.
at each
In order to reduce
temperature. In orderthe test errors,the
to reduce 5 parallel tests5were
test errors, carried
parallel testsout for carried
were each specimen, and
out for each
the average value was taken as the test result.
specimen, and the average value was taken as the test result.

(a) Overall structure of JF150F-II (b) Brake system of JF150F-II

Figure 5. JF150F-II
Figure 5. JF150F-II constant-speed
constant-speed tester.
tester.

µµ was defined as COF using Equation (1), SWR of volume loss of ∆V

ΔV was calculated
according to Equation (2).
f
µ= 𝑓 (1)
𝜇 =FN (1)
𝐹
1 A d1 − d2
∆V = · · (2)
2· π ·r N f
where f was the friction force between the specimen and brake disc (N); FN was the force
generated by normal pressure on the surface (N); r was the distance from the specimen
 1 𝐴 𝑑 −𝑑
∆𝑉 = · · (2)
2·𝜋·𝑟 𝑁 𝑓
Polymers 2023, 15, 4732 7 of 14
where f was the friction force between the specimen and brake disc (N); FN was the force
generated by normal pressure on the surface (N); r was the distance from the specimen
center to the brake disc center (r = 0.15 m); n was the number of revolutions (n = 5000); A
center to the brake disc center (r = 0.15 m); n was the number of revolutions (n = 5000);
was the contact surface area, which was 625 mm2; d1 and d2 were the initial and final thick-
A was the contact surface area, which was 625 mm2 ; d1 and d2 were the initial and final
ness of the specimen (mm), respectively.
thickness of the specimen (mm), respectively.
Due to
Due tothe
thefrequent
frequentor orhard
hardbraking,
braking, the thereduction
reduction ininCOF
COFcaused
caused by
bythe
theincreasing
increasing
interface temperature was known as fade; after the release of brakes
interface temperature was known as fade; after the release of brakes and cooling down, and cooling down,
the extent of revival of the original magnitude of COF was referred to
the extent of revival of the original magnitude of COF was referred to as recovery [29,30]. as recovery [29,30].
The fade
The fade ratio
ratio (F
(Ffade ) and recovery ratio (Frecovery) were calculated by Equation (3) and Equa-
fade ) and recovery ratio (Frecovery ) were calculated by Equation (3) and
tion (4), respectively.
Equation (4), respectively.
𝜇 ℃−𝜇 ℃
𝐹 =
µ F100 ◦ C − µ F350 ◦ C · 100% (3)
Ff ade = 𝜇 ℃ ·100% (3)
µ F100 ◦ C
𝜇
𝐹 =µ R100 · 100% (4)
Frecovery = 𝜇 ·100% (4)
µ F100
where µF100 °C was COF at 100 ℃ during the fade test, µF350 °C was COF at 350 ℃ during the
where µF100 ◦ C was COF at 100 ◦ C during the fade test, µF350 ◦ C was COF at 350 ◦ C during
fade test, and µR100 °C was COF at 100 ℃ during the recovery test.
the fade test, and µR100 ◦ C was COF at 100 ◦ C during the recovery test.
After the friction-wear test, the worn surface morphology was evaluated by a scan-
After the friction-wear test, the worn surface morphology was evaluated by a scanning
ning electron microscope (SEM, EVO-18, ZEISS, Jena, Germany). The samples for SEM
electron microscope (SEM, EVO-18, ZEISS, Jena, Germany). The samples for SEM tests
tests were
were carefullycarefully
cut into cut 5into
mm 5 mm× 5 ×mm5 mm sections
sections perpendicular
perpendicular totoworn
wornsurface
surfaceusing
usingaa
cutterbar (JF151F, Wangda, Changchun, China), which would not
cutterbar (JF151F, Wangda, Changchun, China), which would not destroy the worn surface destroy the worn sur-
morphology, and a thin layer of gold dust was coated on the worn surface using a carbona
face morphology, and a thin layer of gold dust was coated on the worn surface using
carbon(SBC-12,
coater coater (SBC-12, KYKY Technology,
KYKY Technology, Beijing,toChina)
Beijing, China) ensuretothe
ensure the conductivity
conductivity [31]. [31].

3. Results
3. Results and
and Discussion
Discussion
3.1.
3.1. Thermogravimetric
Thermogravimetric Analysis
Analysis
The
The thermographs of
thermographs of PFS-0
PFS-0 andand PFS-8
PFS-8 are
are shown
shown in
in Figure
Figure6. 6. ItIt can
canbebeinferred
inferredthat
that
PFS-0 ◦
100℃,C,
PFS-0 and
and PFS-8 showed
showed the
the first
firstweight
weightloss
lossbelow
below100 which
which cancan be be attributed
attributed to
to the
the water
water evaporation
evaporation or dehydration
or dehydration of water
of water molecules
molecules in the
in the samples
samples [32].[32]. Between
Between 100
100 ◦ C, the weight loss of PFS-0 was higher than that of PFS-8; with temperature
andand225225
℃, the weight loss of PFS-0 was higher than that of PFS-8; with temperature con-
continuously increasing (from ◦
tinuously increasing (from 225225
to to
400400
°C),C),
thethe weight
weight loss
loss of of PFS-8
PFS-8 was was higher
higher than
than that
that of
of PFS-0, which was mainly caused by the cross-linking reaction between
PFS-0, which was mainly caused by the cross-linking reaction between the PEEK fiber and the PEEK fiber
and phenolic
phenolic resin.
resin.

Figure6.6. TGA
Figure TGAcurve
curve of
ofPFS-0
PFS-0and
andPFS-8.
PFS-8.

3.2. Density and Hardness

Figure 7a presents the density of RBFMs strengthened by PEEK fiber. It can be
observed that the density of specimens decreased with the increasing PEEK fiber content,
which could be ascribed to the replacement of low-density PEEK fiber with high-density
barium sulfate. Among all samples, PFS-0 had the maximum density and PFS-8 had the
minimum density.
 minimum density.
3.2. Density and Hardness
Figure 7b shows the hardness of RBFMs strengthened by PEEK fiber. It can be in-
Figure
ferred that with7athe
presents the content
increasing density of
ofPEEK
RBFMs strengthened
fiber, by PEEK
hardness showed fiber. It can
a decreasing be ob-
trend,
served that the density of specimens decreased with the increasing PEEK
which might be caused by the low hardness of the PEEK fiber. Samples presented a hard-fiber content,
Polymers 2023, 15, 4732 which
ness could
in the beofascribed
range to theHRR.
113.3–117.3 replacement of low-density
Furthermore, PEEKthe
on the whole, fiber with high-density
hardness of speci-
8 of 14
barium sulfate. Among all samples, PFS-0 had
mens with different PEEK fiber content changed slightly. the maximum density and PFS-8 had the
minimum density.
Figure 7b shows the hardness of RBFMs strengthened by PEEK fiber. It can be in-
ferred that with the increasing content of PEEK fiber, hardness showed a decreasing trend,
which might be caused by the low hardness of the PEEK fiber. Samples presented a hard-
ness in the range of 113.3–117.3 HRR. Furthermore, on the whole, the hardness of speci-
mens with different PEEK fiber content changed slightly.

(a) Density of RBFMs (b) Hardness of RBFMs

Figure 7. 7.
Figure Density and
Density hardness
and ofof
hardness RBFMs strengthened
RBFMs byby
strengthened PEEK fiber.
PEEK fiber.

Figure
3.3. Impact 7b shows the hardness of RBFMs strengthened by PEEK fiber. It can be inferred
Strength
thatImpact
with the increasing
strength is the content
impact ofresistance
PEEK fiber, ofhardness showed a decreasing
friction materials, which can trend, be used which
to
might be caused
evaluate the toughness by theandlow hardness of the PEEK fiber. Samples presented fiber on me-in
a hardness
(a) Density ofbrittleness
RBFMs [15]. To confirm the(b) influence
Hardness of PEEK
of RBFMs
the range of 113.3–117.3 HRR. Furthermore, on the whole, the hardness of specimens with
chanical properties of RBFMs, the impact strength was evaluated by an impact tester. Fig-
Figure 7. PEEK
different Densityfiber
and content
hardnesschanged
of RBFMsslightly.
strengthened by PEEK fiber.
ure 8 presents the impact strength of RBFMs with different PEEK fiber content. It could
be3.3.
inferred that the PEEK fiber could enhance the impact strength of RBFMs. The impact
3.3.Impact
ImpactStrength
Strength
strength showed an increasing at first and then a decreasing trend with increasing PEEK
Impact strength
ImpactPFS-6strength is the impact
impactresistance of
offriction materials, which can
canbe used to
fiber content. had is thethe maximum resistance
impact strength friction
amongmaterials,
all sampleswhich (0.362 be
J/mmused 2), to
evaluate
evaluate the
the toughness and and brittleness
brittleness[15].
[15].ToToconfirm
confirm the
the influence
influence of of PEEK
PEEK fiber
fiber on on
me-
which was 9.04% higher than that of PFS-0. The enhanced impact strength could be at-
mechanical
chanical properties
properties of RBFMs, the impact strengthwaswas evaluated byimpact
an impact tester.
tributed to the bearingofcapacity
RBFMs, thePEEK
of impact strength
fiber [15]; during evaluated
the impact by process,
an tester.
the PEEK Fig-
Figure
urecan 8 presents
8 presents the impact strength of RBFMs with different PEEK fiber content. It could
fiber not onlythe bearimpact
the stressstrength of RBFMs
in RBFMs with
but also different
transfer andPEEK fiberthe
disperse content. It could
stress more
be
be inferred
inferred that
thatthe
the PEEK
PEEK fiber
fiber could
could enhance
enhance the
the impact
impact strength
strength ofofRBFMs.
RBFMs. The
The impact
impact
effectively, thus showing an improved impact strength [7,17].
strength
strength showed an increasing at first and then a decreasing trend with increasingPEEK
showed an increasing at first and then a decreasing trend with increasing PEEK
fiber 2
fibercontent.
content.PFS-6
PFS-6had hadthe themaximum
maximumimpact impactstrength
strengthamong
amongall allsamples
samples(0.362
(0.362J/mm
J/mm2),),
which
whichwas was 9.04%
9.04% higher
higher than that of
than that of PFS-0.
PFS-0. The Theenhanced
enhancedimpactimpact strength
strength could
could be be
at-
attributed to the bearing capacity of PEEK fiber [15]; during the
tributed to the bearing capacity of PEEK fiber [15]; during the impact process, the PEEKimpact process, the PEEK
fiber
fibercan
cannotnotonly
onlybear
bearthe thestress
stressininRBFMs
RBFMsbut butalso
alsotransfer
transferandanddisperse
dispersethe thestress
stressmore
more
effectively, thus showing an improved impact
effectively, thus showing an improved impact strength [7,17]. strength [7,17].

Figure 8. Impact strength of RBFMs strengthened by PEEK fiber.

Figure8.8.Impact
Figure Impactstrength
strengthofofRBFMs
RBFMsstrengthened
strengthenedby
byPEEK
PEEKfiber.
fiber.

3.4. Tribological Properties

Figure 9 presents the COF of RBFMs with different amounts of PEEK fiber at the
normal pressure and sliding velocity of 0.98 MPa and 7.536 m/s, respectively. As seen in
Figure 9a, the introduction of PEEK fiber caused a reduction in COF. At different braking
temperatures, samples holding PEEK fiber exhibited a smaller COF. Indeed, the high
strength, high modulus and the formation of immobilized interfacial zone around the
PEEK fiber can cause the dissipation of a major portion of braking stress exerted during
braking, thus reducing the COF [15]. Moreover, the introduction of PEEK fiber can not
 Figure 9 presents the COF of RBFMs with different amounts of PEEK fiber at the
normal pressure and sliding velocity of 0.98 MPa and 7.536 m/s, respectively. As seen in
Figure 9a, the introduction of PEEK fiber caused a reduction in COF. At different braking
temperatures, samples holding PEEK fiber exhibited a smaller COF. Indeed, the high
Polymers 2023, 15, 4732
strength, high modulus and the formation of immobilized interfacial zone around9 the of 14

PEEK fiber can cause the dissipation of a major portion of braking stress exerted during
braking, thus reducing the COF [15]. Moreover, the introduction of PEEK fiber can not
onlyenhance
only enhancethethemechanical
mechanicalproperties
propertiesof
ofRBFMs
RBFMsbutbutalso
alsoreduce
reduceCOF
COFand
andSWR
SWRbecause
because
of its self-lubricating property [33]. During the fade test, PFS-2 showed the slightest COF
of its self-lubricating property [33]. During the fade test, PFS-2 showed the slightest COF
variation among all samples with increasing braking temperatures, which obtained the
variation among all samples with increasing braking temperatures, which obtained◦ the
optimal COF stability. Furthermore, Figure 9b shows the braking curves at 350 C; it
optimal COF stability. Furthermore, Figure 9b shows the braking curves at 350 °C; it can
can be inferred in Figure 9b that PFS-2 had the most stable braking process at the same
be inferred in Figure 9b that PFS-2 had the most stable braking process at the same tem-
temperature (350 ◦ C), where there was no obvious braking instability.
perature (350 °C), where there was no obvious braking instability.

(a) COF at fade test (b) Braking curves

(c) COF at recovery test (d) Fade ratio and recovery ratio
Figure
Figure9.9.COF
COFofofRBFMs
RBFMsstrengthened
strengthenedby
byPEEK
PEEKfiber.
fiber.

Asrevealed
As revealedby byFigure
Figure9a, 9a,the
theCOF
COFof ofPFS-0
PFS-0(with
(withPEEKPEEKfiber
fiberof
of00wt.%)
wt.%)experienced
experienced
anincrease
an increaseatatfirst
firstand
andthenthenaadecreasing
decreasingtrend trendwith
withthe the increase
increase inin temperature.
temperature.This Thisisis
consistentwith
consistent withthe
theprevious
previous results
results [21].
[21]. AApossible
possibleexplanation
explanationofofthe theincreasing
increasingCOF COF
between 100
between 100 and 200 ◦°C C was
was that
thatthetheexposed
exposedfibers fibers(such
(such asas
PEEK
PEEKfiber, sepiolite
fiber, fiber,
sepiolite and
fiber,
compound mineral fibers) on the friction surface would scrape
and compound mineral fibers) on the friction surface would scrape the brake disc, which the brake disc, which was
transformed
was intointo
transformed friction output
friction output[34].[34].
WithWith the further
the furtherincreasing in braking
increasing temperature,
in braking temper-
the COF
ature, begun
the COF to reduce,
begun which
to reduce, could
which be attributed
could be attributed to the decreasing
to the decreasing shear
shearstrength
strength of
phenolic
of phenolic resin at at
resin higher
higher temperatures
temperatures [2].[2].
In In
addition,
addition, thethe
lubrication
lubricationcomponents
components from
fromthe
degradation
the degradationof phenolic
of phenolic resin at high
resin at hightemperatures
temperatures could also
could cause
also causea decreased
a decreased COFCOF[3].
Interestingly, the behaviors of samples holding PEEK fiber were quite
[3]. Interestingly, the behaviors of samples holding PEEK fiber were quite different. Spe- different. Specifically,
specimens
cifically, having less
specimens havingPEEK lessfiber
PEEK (2fiber
wt.%(2and wt.% 4 wt.%) reported
and 4 wt.%) a COFa decreasing
reported COF decreasingtrend
with the increasing temperature, while specimens holding more
trend with the increasing temperature, while specimens holding more PEEK fiber (6 wt.% PEEK fiber (6 wt.% and
8 wt.%) showed a COF variation trend of increasing from 100 to 150 ◦ C, dropping from 150
and 8 wt.%) showed a COF variation trend of increasing from 100 to 150 °C, dropping
to 300 ◦ ◦
from 150Ctoand
300increasing again from
°C and increasing 300from
again to 350 300Cto(shown
350 °Cin Figurein9a).
(shown Figure 9a).
Figure 9c shows the COF in the recovery test. It served to show that the self-lubrication
property of the PEEK fiber could still reduce COF with decreasing temperatures. The COF
of PFS-0 (incorporating PEEK fiber of 0 wt.%) kept a higher COF at different braking
temperatures. The COF of PFS-0 exhibited an increase at first and then a decreasing trend
with reducing braking temperatures; the COF of PFS-2 and PFS-4 kept increasing with
decreasing braking temperatures; whereas PFS-6 had the opposite trend with that of PFS-2
and PFS-4; finally, PFS-8 showed a COF variation trend of increasing firstly and then
remained stable.
 tion property of the PEEK fiber could still reduce COF with decreasing temperatures. The
COF of PFS-0 (incorporating PEEK fiber of 0 wt.%) kept a higher COF at different braking
temperatures. The COF of PFS-0 exhibited an increase at first and then a decreasing trend
with reducing braking temperatures; the COF of PFS-2 and PFS-4 kept increasing with
Polymers 2023, 15, 4732 decreasing braking temperatures; whereas PFS-6 had the opposite trend with that of10PFS- of 14
2 and PFS-4; finally, PFS-8 showed a COF variation trend of increasing firstly and then
remained stable.
To
To further
furtherevaluate
evaluatethe theCOFCOFvariation,
variation, it made
it made sense to determine
sense to determine the fade
the faderatioratio
and
recovery ratio. As evident from Figure 9d, the fade ratio order
and recovery ratio. As evident from Figure 9d, the fade ratio order was PFS-4 > PFS-6 > was PFS-4 > PFS-6 > PFS-2
>PFS-2
PFS-0> >PFS-0
PFS-8; the result
> PFS-8; showed
the result that PFS-8
showed (incorporating
that PFS-8 (incorporating PEEKPEEK fiber offiber8 wt.%) had
of 8 wt.%)
the optimal fade ratio (1.92%), which had a better fade resistance
had the optimal fade ratio (1.92%), which had a better fade resistance than that of Farhad than that of Farhad Ah-
madijokani
Ahmadijokani [12][12]
andand
AmarAmar Patnaik
Patnaik [35] reported.
[35] reported. AsAs illustrated
illustratedininFigure
Figure9d, 9d,the therecovery
recovery
ratio
ratio order
order waswas PFS-8
PFS-8 >> PFS-2
PFS-2 >> PFS-0
PFS-0 >>PFS-6PFS-6 >>PFS-4,
PFS-4,and andPFS-6
PFS-6 obtained
obtained the the first-rank
first-rank
recovery
recovery property
property (100%).
(100%). Interestingly,
Interestingly, PFS-2PFS-2 alsoalso had
had aa better
better recovery
recovery ratioratio of of 113.94%.
113.94%.
Summing up the above, the incorporation of PEEK fiber
Summing up the above, the incorporation of PEEK fiber could improve tribologi- could improve tribological
properties of RBFMs.
cal properties of RBFMs.Comparing
Comparing samples holding
samples different
holding contentcontent
different of PEEK of fiber,
PEEKPFS-2fiber,
had
PFS-2thehad
morethe outstanding
more outstanding fade resistance
fade resistanceand recovery
and recovery property, and itand
property, haditmorehad morepro-
nounced
pronounced friction stability
friction during
stability the the
during whole whole test.test.
The
The composition
composition and and fabrication
fabrication process
process can can influence
influence the thewear
wearresistance
resistanceof ofRBFMs,
RBFMs,
which
which finally
finally determines
determines the the service
service life
life [36].
[36]. InIn this
this study,
study, the wear wear resistance
resistance of of RBFMs
RBFMs
incorporating different PEEK fiber content was evaluated by
incorporating different PEEK fiber content was evaluated by comparing SWR at different comparing SWR at different
braking
braking temperatures
temperatures and the the sum
sum of of SWR.
SWR. Figure
Figure 10a10a displayed
displayed the the SWR
SWR variation
variation trendtrend
at different
at differentbraking
brakingtemperatures.
temperatures. TheThefriction-wear
friction-wear test demonstrated
test demonstrated that SWR thatofSWR RBFMs of
was remarkable
RBFMs affected affected
was remarkable by PEEKby fiber;
PEEK the fiber;
SWR the of samples
SWR ofholding samplesPEEK holdingfiberPEEK
was lower
fiber
thanlower
was that ofthan
PFS-0thatespecially at high temperatures;
of PFS-0 especially moreover, moreover,
at high temperatures; it increasedit with increasing
increased with
braking temperature. Our results showed similar trends with
increasing braking temperature. Our results showed similar trends with the reported the reported work of Yucheng
Liu [21].
work SWR observably
of Yucheng Liu [21]. increased
SWR observably with increasing
increasedtemperature
with increasing 250 to 350 ◦from
fromtemperature C. In
250 to 350 ℃. In this temperature range, the bonding strength between phenolic resin
this temperature range, the bonding strength between phenolic resin binder and other
reinforcement
binder and other composition
reinforcement wascomposition
weakened, which resulted from
was weakened, which the thermal
resulted fromdegradation
the ther-
of phenolic
mal degradationresinof matrix
phenolic[37,38],
resinthus significantly
matrix [37,38], thus reducing the shearing
significantly reducing strength [2]. In
the shearing
addition, the glass transition of PEEK fiber also occurred in this
strength [2]. In addition, the glass transition of PEEK fiber also occurred in this tempera- temperature range [25],
which would also cause an increscent SWR. Figure 10b
ture range [25], which would also cause an increscent SWR. Figure 10b showed the sumshowed the sum of SWR at each
temperature.
of SWR at each It temperature.
could be inferred thatbe
It could theinferred
incorporation
that theofincorporation
PEEK fiber can of reduce
PEEK fiber the sum
can
of SWR by 13.51%–52.86% and PFS-6 had the optimal
reduce the sum of SWR by 13.51%–52.86% and PFS-6 had the optimal wear resistance. wear resistance. Furthermore, the
wear resistance of RBFMs strengthened by PEEK fiber
Furthermore, the wear resistance of RBFMs strengthened by PEEK fiber was higher thanwas higher than that of RBFMs
strengthened
that of RBFMsby glass fiber [39],
strengthened jute fiber
by glass fiber [40]
[39],and
jutecorn
fiberstalk
[40] fiber
and corn [21].stalk fiber [21].

(a) SWR at different temperatures (b) The sum of SWR at different temperatures
Figure
Figure 10.
10. SWR
SWR of
of RBFMs
RBFMs strengthened
strengthened by
by PEEK
PEEK fiber.
fiber.

In conclusion, the
In conclusion, thepromoted
promotedwear
wearresistance
resistance
of of RBFMs
RBFMs by PEEK
by PEEK fiberfiber could
could be as-
be ascribed
cribed to the bearing function at lower temperatures and the adhesion function
to the bearing function at lower temperatures and the adhesion function of wear debrisof wearat
high temperatures to facilitate the formation of secondary plateau [25]. Additionally, the
PEEK fiber can form a layer of lubrication film because of its self-lubrication properties,
which can also reduce abrasion [27].

3.5. Wear Mechanisms

Primary and secondary plateaus, adhesive pits, wear debris and grooves on worn
surface can be used to analyze the wear mechanisms of friction materials [41]. The worn
 tionally, the PEEK fiber can form a layer of lubrication film because of its self-lubrication
properties, which can also reduce abrasion [27].

3.5. Wear Mechanisms

Polymers 2023, 15, 4732
Primary and secondary plateaus, adhesive pits, wear debris and grooves on11worn of 14
surface can be used to analyze the wear mechanisms of friction materials [41]. The worn
surface morphology was characterized by SEM to analyze wear mechanisms, thus obtain-
surface
ing themorphology
mechanism was characterized
for the by SEM
improved wear to analyze
resistance by wear
PEEKmechanisms,
fiber. thus obtaining
the mechanism for the improved wear resistance by PEEK fiber.
As observed in Figure 11a, a large amount of wear debris and pits were found, indi-
Asthat
cating observed in mechanisms
the wear Figure 11a, awere
largesevere
amount of wear
abrasive weardebris and pits were
and adhesive found,
wear [5]. in-
In fact,
dicating that the wear mechanisms were severe abrasive wear and adhesive
the composition of RBFMs can determine wear resistance and then influence its wear wear [5]. In
fact, the composition of RBFMs can determine wear resistance and then influence
mechanisms [38]. The serious abrasion of samples incorporating no PEEK fiber can be its wear
mechanisms
attributed to[38].
the The
lack serious abrasion ofeffect
of strengthening samples
and incorporating
self-lubricationnofilm
PEEK byfiber
PEEK canfiber
be
attributed
[21,42]. to the lack of strengthening effect and self-lubrication film by PEEK fiber [21,42].

(a) PEEK fiber content of 0 wt.% (b) PEEK fiber content of 2 wt.%

(c) PEEK fiber content of 4 wt.% (d) PEEK fiber content of 6 wt.%

(e) PEEK fiber content of 8 wt.%

Figure11.
Figure 11.Worn
Wornsurface
surfacemorphology
morphologyofofRBFMs
RBFMsstrengthened
strengthenedby
byPEEK
PEEKfiber.
fiber.

The PEEK fiber in RBFMs mainly played a bearing and self-lubrication role at lower
braking temperatures. While the braking temperature was more than its melting point of
343 ◦ C, the molten PEEK fiber would adhere to wear debris on a worn surface to reduce
abrasive wear; and under the action of normal pressure, the adhered wear debris would
form a secondary plateau, which can protect friction materials from being hurt by wear
debris and the brake disc (shown in Figure 12). Figure 11b–e present the worn surface
morphology of RBFMs incorporating different content of PEEK fiber. It served to show that
the wear mechanisms of RBFMs holding less PEEK fiber (2 wt.%) were mainly abrasive
wear and adhesive wear; there were some wear debris, plastic deformation and little
 343 °C, the molten PEEK fiber would adhere to wear debris on a worn surface to reduce
abrasive wear; and under the action of normal pressure, the adhered wear debris would
form a secondary plateau, which can protect friction materials from being hurt by wear
debris and the brake disc (shown in Figure 12). Figure 11b–e present the worn surface
Polymers 2023, 15, 4732 morphology of RBFMs incorporating different content of PEEK fiber. It served to12show of 14
that the wear mechanisms of RBFMs holding less PEEK fiber (2 wt.%) were mainly abra-
sive wear and adhesive wear; there were some wear debris, plastic deformation and little
primary
primaryand
andsecondary
secondaryplateaus
plateauson
onworn
wornsurface.
surface.ItItalso
alsoserved
servedto
toshow
showin
inFigure
Figure11b
11bthat
that
aalower
lowercontent
content of
ofPEEK
PEEKfiber
fibercannot
cannotachieve
achieveeffective
effective adhesion
adhesion to
towear
weardebris;
debris; thus,
thus, itit
presented
presentedaarelatively
relativelyrough
roughworn
wornsurface.
surface.

Figure12.
Figure 12.Wear
Wearmechanism
mechanismof
ofRBFMs
RBFMsstrengthened
strengthenedby
byPEEK
PEEKfiber
fiberatathigh
hightemperatures.
temperatures.

With
Withincreasing
increasingPEEKPEEKfiber
fibercontent
content (4–6 wt.%),
(4–6 wt.%), a large amount
a large of wear
amount of weardebris was was
debris ad-
hered by molten PEEK and was compacted as the secondary plateau,
adhered by molten PEEK and was compacted as the secondary plateau, which was mani- which was manifested
as a more
fested as asmooth worn surface
more smooth worn (shown in Figurein11c,d).
surface (shown FigureThere
11c,d). was a little
There wasamount
a little of wear
amount
debris
of wearand pits on
debris andthe worn
pits on surface;
the wornmeanwhile, a large amount
surface; meanwhile, a largeof amount
primary of and secondary
primary and
plateaus
secondarycould be observed.
plateaus could be Generally speaking, speaking,
observed. Generally the primary theplateau
primarywas composed
plateau was com- of
components with higher
posed of components mechanical
with strength and
higher mechanical better wear
strength resistance
and better wear(such as reinforced
resistance (such as
fibers and hard
reinforced particles)
fibers and hard [34,43], and these
particles) [34,43],primary
and theseplateaus
primaryacted as a barrier,
plateaus actedreducing the
as a barrier,
movement of wear debris, making them tend to stop and stick together
reducing the movement of wear debris, making them tend to stop and stick together on on the worn surface
and be compacted,
the worn surface and thus
be promoting
compacted,the thusformation
promoting of the
a secondary
formationplateau [44–46].plateau
of a secondary Many
studies
[44–46].have
Many shown thathave
studies the formation
shown that of athe
secondary
formation plateau on worn surfaces
of a secondary plateauplayed
on wornan
important role inan
surfaces played improving
importanttribological properties
role in improving [39,47]. With
tribological the PEEK
properties fiberWith
[39,47]. content
the
continuously increasing
PEEK fiber content (8 wt.%), the
continuously thermoplastic
increasing PEEKthe
(8 wt.%), and thermosettingPEEK
thermoplastic phenolic
and resin
ther-
were cross-linked and cured under high temperatures, which
mosetting phenolic resin were cross-linked and cured under high temperatures, caused a reduction inwhich
wear
resistance, showing ainmore
caused a reduction wearrough worn surface.
resistance, showingThis a morewasrough
in agreement with our
worn surface. previous
This was in
study [25].
agreement with our previous study [25].
4. Conclusions
4. Conclusions
To overcome the disadvantages of lacking adaptive capacity to different braking
To overcome the disadvantages of lacking adaptive capacity to different braking con-
conditions of traditional RBFMs, a new RBFM strengthened by PEEK fiber was developed,
ditions of traditional RBFMs, a new RBFM strengthened by PEEK fiber was developed,
which provided a novel idea for the research of intelligent friction materials. The mechanical
which provided a novel idea for the research of intelligent friction materials. The mechan-
and tribological properties can be effectively regulated by the content of PEEK fiber. The
ical andstrength
impact tribological properties can
and tribological be effectively
properties regulated
were not by theimproved
significantly content ofwith
PEEK fiber.
a lower
content of PEEK fiber (2 wt.%). With the increase in PEEK fiber content (4 wt.%), the impacta
The impact strength and tribological properties were not significantly improved with
lower content
strength and wearof PEEK fiber (2
resistance wt.%). With
increased thethe
due to increase in PEEKand
high strength fiberself-lubrication
content (4 wt.%),
of
the impact
PEEK fiber;strength
however, andthewear
faderesistance
resistanceincreased dueAs
decreased. tothe
thePEEK
high strength and self-lubri-
fiber content reached
cation
to of PEEK
6 wt.%, samplesfiber; however,
showed the fadecomprehensive
the optimal resistance decreased. As the PEEK
performances. Withfiber
PEEK content
fiber
reached to 6 wt.%, samples showed the optimal comprehensive performances.
continuously increasing (8 wt.%), its comprehensive properties began to decline to a certainWith PEEK
fiber continuously
extent. Furthermore, increasing
chemical(8 wt.%), its comprehensive
enhancement on PEEK fiberproperties
might be began to decline to
also worthwhile fora
enhancing the comprehensive performances of RBFMs [48], and we will investigate the
influences of chemical treatment for PEEK fiber on dielectric, thermal, mechanical and
tribological properties of RBFMs in the future.

Author Contributions: L.L.: Conceptualization, Methodology, Investigation, Validation, Data cu-

ration, Writing—original draft, Z.M.: Investigation, Validation, Writing—review and editing, G.L.:
Investigation, Validation, Writing—review and editing, W.S.: Investigation, Validation, Writing—
review and editing, L.R.: Conceptualization, S.Y.: Methodology, X.Y.: Writing—review and editing,
Polymers 2023, 15, 4732 13 of 14

Q.Z.: Investigation, Validation, Methodology and Supervision, Y.M.: Funding acquisition, Resources,
Project administration. All authors have read and agreed to the published version of the manuscript.
Funding: This study was funded by the National Natural Science Foundation of China (No. 52275288),
Jilin Province Science and Technology Development Plan Item (No. 20210202021NC), Changchun City
Science and Technology Development Plan Item (No. 21ZGN15), Jilin Scientific and Technological
Development Program (No. 20230508019RC).
Institutional Review Board Statement: Not applicable.
Data Availability Statement: Data are contained within the article.
Conflicts of Interest: The authors declare no conflict of interest.

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