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Graphene-Polymer
Composites II
Edited by
Artur Pinto and Fernão D. Magalhães
Printed Edition of the Special Issue Published in Polymers
Graphene-Polymer Composites II
Graphene-Polymer Composites II

Editors
Artur Pinto
Fernão D. Magalhães

MDPI • Basel • Beijing • Wuhan • Barcelona • Belgrade • Manchester • Tokyo • Cluj • Tianjin
Editors
Artur Pinto Fernão D. Magalhães
University of Porto University of Porto
Portugal Portugal

Editorial Office
MDPI
St. Alban-Anlage 66
4052 Basel, Switzerland

This is a reprint of articles from the Special Issue published online in the open access journal Polymers
(ISSN 2073-4360) (available at: www.mdpi.com/journal/polymers/special issues/Graphene Polym
Compos II).

For citation purposes, cite each article independently as indicated on the article page online and as
indicated below:

LastName, A.A.; LastName, B.B.; LastName, C.C. Article Title. Journal Name Year, Volume Number,
Page Range.

ISBN 978-3-0365-1678-3 (Hbk)

ISBN 978-3-0365-1677-6 (PDF)

© 2021 by the authors. Articles in this book are Open Access and distributed under the Creative
Commons Attribution (CC BY) license, which allows users to download, copy and build upon
published articles, as long as the author and publisher are properly credited, which ensures maximum
dissemination and a wider impact of our publications.
The book as a whole is distributed by MDPI under the terms and conditions of the Creative Commons
license CC BY-NC-ND.
Contents

About the Editors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . vii

Preface to ”Graphene-Polymer Composites II” . . . . . . . . . . . . . . . . . . . . . . . . . . . . ix

Artur M. Pinto and Fernão D. Magalhães

Graphene-Polymer Composites *
Reprinted from: Polymers 2021, 13, 685, doi:10.3390/polym13050685 . . . . . . . . . . . . . . . . . 1

Alaeddin Burak Irez, Emin Bayraktar and Ibrahim Miskioglu

Fracture Toughness Analysis of Epoxy-Recycled Rubber-Based Composite Reinforced with
Graphene Nanoplatelets for Structural Applications in Automotive and Aeronautics
Reprinted from: Polymers 2020, 12, 448, doi:10.3390/polym12020448 . . . . . . . . . . . . . . . . . 7

S. S. R. Koloor, S. M. Rahimian-Koloor, A. Karimzadeh, M. Hamdi, Michal Petrů and M. N.

Tamin
Nano-Level Damage Characterization of Graphene/Polymer Cohesive Interface under Tensile
Separation
Reprinted from: Polymers 2019, 11, 1435, doi:10.3390/polym11091435 . . . . . . . . . . . . . . . . 23

Chengguo Liu, Cuina Wang, Jijun Tang, Jing Zhang, Qianqian Shang, Yun Hu, Hongxiao
Wang, Qiong Wu, Yonghong Zhou, Wen Lei and Zengshe Liu
High-Performance Biobased Unsaturated Polyester Nanocomposites with Very Low Loadings
of Graphene
Reprinted from: Polymers 2018, 10, 1288, doi:10.3390/polym10111288 . . . . . . . . . . . . . . . . 39

Feng Yang, Cuiqin Lan, Haiming Zhang, Jian Guan, Fan Zhang, Benhua Fei and Jilei Zhang
Study on Graphene/CNC-Coated Bamboo Pulp Fabric Preparation of Fabrics with Thermal
Conductivity
Reprinted from: Polymers 2019, 11, 1265, doi:10.3390/polym11081265 . . . . . . . . . . . . . . . . 53

Hooman Abbasi, Marcelo Antunes and José Ignacio Velasco

Effects of Graphene Nanoplatelets and Cellular Structure on the Thermal Conductivity of
Polysulfone Nanocomposite Foams
Reprinted from: Polymers 2019, 12, 25, doi:10.3390/polym12010025 . . . . . . . . . . . . . . . . . 65

Lijie Zhou, Shengcheng Zhai, Yiming Chen and Zhaoyang Xu

Anisotropic Cellulose Nanofibers/Polyvinyl Alcohol/Graphene Aerogels Fabricated by
Directional Freeze-drying as Effective Oil Adsorbents
Reprinted from: Polymers 2019, 11, 712, doi:10.3390/polym11040712 . . . . . . . . . . . . . . . . . 81

Chien-Lin Huang, Hsuan-Hua Wu, Yung-Ching Jeng and Wei-Zhi Liang

Electrospun Graphene Nanosheet-Filled Poly(Trimethylene Terephthalate) Composite Fibers:
Effects of the Graphene Nanosheet Content on Morphologies, Electrical Conductivity,
Crystallization Behavior, and Mechanical Properties
Reprinted from: Polymers 2019, 11, 164, doi:10.3390/polym11010164 . . . . . . . . . . . . . . . . . 97

Justin W. Hendrix, Ryan Szeto, Thomas Nosker, Jennifer Lynch-Branzoi and Thomas J. Emge
Evaluation of Exfoliated Graphite to Graphene in Polyamide 66 Using Novel High Shear
Elongational Flow
Reprinted from: Polymers 2018, 10, 1399, doi:10.3390/polym10121399 . . . . . . . . . . . . . . . . 121

v
Miao Miao, Chunyan Wei, Ying Wang and Yongfang Qian
Effect of Compatibilizer on the Interface Bonding of Graphene Oxide/Polypropylene
Composite Fibers
Reprinted from: Polymers 2018, 10, 1283, doi:10.3390/polym10111283 . . . . . . . . . . . . . . . . 135

Yanhua Lei, Zhichao Qiu, Jiurong Liu, Dongdong Li, Ning Tan, Tao Liu, Yuliang Zhang,
Xueting Chang, Yanhong Gu and Yansheng Yin
Effect of Conducting Polyaniline/Graphene Nanosheet Content on the Corrosion Behavior of
Zinc-Rich Epoxy Primers in 3.5% NaCl Solution
Reprinted from: Polymers 2019, 11, 850, doi:10.3390/polym11050850 . . . . . . . . . . . . . . . . . 145

Sangiliyandi Gurunathan, Muniyandi Jeyaraj, Min-Hee Kang and Jin-Hoi Kim

Graphene Oxide–Platinum Nanoparticle Nanocomposites: A Suitable Biocompatible
Therapeutic Agent for Prostate Cancer
Reprinted from: Polymers 2019, 11, 733, doi:10.3390/polym11040733 . . . . . . . . . . . . . . . . . 161

Raquel Costa-Almeida, Diana Bogas, José R. Fernandes, Licı́nia Timochenco, Filipa A. L. S.

Silva, João Meneses, Inês C. Gonçalves, Fernão D. Magalhães and Artur M. Pinto
Near-Infrared Radiation-Based Mild Photohyperthermia Therapy of Non-Melanoma Skin
Cancer with PEGylated Reduced Nanographene Oxide
Reprinted from: Polymers 2020, 12, 1840, doi:10.3390/polym12081840 . . . . . . . . . . . . . . . . 185

vi
About the Editors
Artur Pinto graduated in Pharmaceutical Sciences, obtaining his PhD in Biomedical Engineering
from Faculty of Engineering - University of Porto (FEUP), visiting U. Washington. Afterwards, Artur
has been appointed as a Post-Doctoral Researcher at Eindhoven University of Technology, Chemical
Engineering Department, the Netherlands. Following his Post-doc, Artur has been awarded a
long-term Researcher position at LEPABE-FEUP. He is the Principal Investigator of a collaborative
project between FEUP and i3S (Instituto de Investigação e Inovação em Saúde) focused on
developing graphene-based materials and adjusting their properties for biomedical applications,
such as phototherapy of skin disease and cancer and immunotherapy.

Fernão D. Magalhães obtained his PhD in Chemical Engineering from University of

Massachusetts at Amherst, USA, in 1997. He is currently Associate Professor at FEUP, and
senior member of LEPABE, where he leads a research group on Materials Science (polymers,
nanomaterials, and composites). His research interests include synthetic and natural adhesives for
wood and cork based composites, graphene-based materials for biomedical applications, synthesis,
and modification of waterborne polymer dispersions and high-performance industrial coatings.

vii
Preface to ”Graphene-Polymer Composites II”
Graphene-polymer nanocomposites continue to gain interest in diverse scientific and
technological fields. Graphene-based nanomaterials present the advantages of other carbon
nanofillers, like electrical and thermal conductivity, while having significantly lower production costs
when compared to materials such as carbon nanotubes, for instance. In addition, in the oxidized
forms of graphene, the large specific area combined with a large quantity of functionalizable chemical
groups available for physical or chemical interaction with polymers, allow for good dispersion and
tunable binding with the surrounding matrix. Other features are noteworthy in graphene-based
nanomaterials, like their generally good biocompatibility and the ability to absorb near-infrared
radiation, allowing for the use in biomedical applications, such as drug delivery and photothermal
therapy.
This Special Issue provides an encompassing view on the state of the art of graphene-polymer
composites, showing how current research is dealing with new and exciting challenges. The
published papers cover topics ranging from novel production methods and insights on mechanisms
of mechanical reinforcement of composites, to applications as diverse as automotive and aeronautics,
cancer treatment, anticorrosive coatings, thermally conductive fabrics and foams, and oil-adsorbent
aerogels.

Artur Pinto, Fernão D. Magalhães

Editors

ix
 polymers
Editorial
Graphene-Polymer Composites *
Artur M. Pinto and Fernão D. Magalhães

LEPABE—Laboratory for Process Engineering, Environment, Biotechnology and Energy, Faculty of Engineering,
University of Porto, 4200-465 Porto, Portugal; [email protected]
* Correspondence: [email protected]

Graphene-polymer nanocomposites continue to gain interest in diverse scientific and

technological fields. Graphene-based nanomaterials present the advantages of other car-
bon nanofillers, like electrical and thermal conductivity, while having significantly lower
production costs when compared to materials such as carbon nanotubes, for instance.
In addition, in the oxidized forms of graphene, the large specific area combined with a
large quantity of functionalizable chemical groups available for physical and/or chemical
interaction with polymers, allow for good dispersion and tunable binding with the sur-
rounding matrix. Other features are noteworthy in graphene-based nanomaterials, like
their generally good biocompatibility and the ability to absorb NIR radiation, allowing for
the use in biomedical applications, such as drug delivery and photothermal therapy.
This Special Issue provides an encompassing view on the state of the art of graphene-
polymer composites, showing how current research is dealing with new and exciting
challenges. The published papers cover topics ranging from novel production methods
and insights on mechanisms of mechanical reinforcement of composites, to applications as
diverse as automotive and aeronautics, cancer treatment, anticorrosive coatings, thermally
conductive fabrics and foams, and oil-adsorbent aerogels. The most impactful works are
summarized in this editorial.



Taking advantage of graphene’s unique mechanical properties, Irez et al. newly


designed lightweight and cost-efficient composite materials for the aeronautic industry
Citation: Pinto, A.M.; Magalhães,
using recycled fresh scrap rubber, epoxy resin, and graphene nanoplatelets (GnPs). After
F.D. Graphene-Polymer Composites.
manufacturing the composites, their bending strength and fracture characteristics were
Polymers 2021, 13, 685. https://
investigated by three-point bending (3PB) tests. Halpin–Tsai homogenization adapted
doi.org/10.3390/polym13050685
to composites containing GnPs was used to estimate the moduli of the composites, and
satisfactory agreement with the 3PB test results was observed. In addition, 3PB tests were
Received: 19 January 2021
Accepted: 20 February 2021
simulated by the finite element method incorporating the Halpin–Tsai homogenization,
Published: 25 February 2021
and the resulting stress–strain curves were compared with the experimental results. Me-
chanical test results showed that the reinforcement with GnPs generally increased the
Publisher’s Note: MDPI stays neutral
modulus of elasticity as well as the fracture toughness of these novel composites. The
with regard to jurisdictional claims in
typical toughening mechanisms observed were crack deflection and cavity formation.
published maps and institutional affil- Considering the advantageous effects of GnPs on these novel composites and the cost
iations. efficiency gained by the use of recycled rubber, these composites have the potential to
be used to manufacture various components in the automotive and aeronautic industries
as well as smart building materials in civil engineering applications [1]. The mechanical
behavior of graphene/polymer interfaces in the graphene-reinforced epoxy nanocomposite
Copyright: © 2021 by the authors.
is one of the factors that dictates the deformation and damage response of the nanocom-
Licensee MDPI, Basel, Switzerland.
posites. Koloor et al. performed hybrid molecular dynamic (MD) and finite element (FE)
This article is an open access article
simulations of a graphene/polymer nanocomposite to characterize the elastic-damage
distributed under the terms and behavior of graphene/polymer interfaces under a tensile separation condition. The MD
conditions of the Creative Commons results show that the graphene/epoxy interface behaves in the form of an elastic-softening
Attribution (CC BY) license (https:// exponential regressive law. The FE results verified the adequacy of the cohesive zone model
creativecommons.org/licenses/by/ in accurate prediction of the interface damage behavior. The graphene/epoxy cohesive
4.0/). interface was characterized by normal stiffness, tensile strength, and fracture energy of

Polymers 2021, 13, 685. https://doi.org/10.3390/polym13050685 https://www.mdpi.com/journal/polymers

Polymers 2021, 13, 685

5 × 10−8 (aPa nm−1 ), 9.75 × 10−10 (nm), 2.1 × 10−10 (N nm−1 ), respectively, followed by
an exponential regressive law with the exponent, α = 7.74. It was shown that the commonly
assumed bilinear softening law of the cohesive interface could lead up to a 55% error in the
predicted separation of the interface [2].
Using a different resin, Liu et al. prepared graphene-reinforced tung oil (TO)-based
unsaturated polyester nanocomposites via in situ melt polycondensation integrated with
Diels–Alder addition. Functionalized graphene sheets derived from graphene oxide (GO)
were then extracted from the obtained nanocomposites and carefully characterized. The
mechanical and thermal properties of the TO-based unsaturated polyester resin (UPR) were
greatly improved by the incorporation of GO. At the optimal GO content (0.10 wt.%) the
nanocomposite showed a tensile strength and a tensile modulus of 43.2 MPa and 2.62 GPa,
and Tg of 105.2 ◦ C, which were 159%, 191%, and 49.4% higher than those of the unreinforced
UPR/TO resin, respectively. Compared to neat UPR, the biobased UPR nanocomposite
with 0.10 wt.% of GO even demonstrated superior comprehensive properties (comparable
stiffness and Tg , while better toughness and thermal stability). Therefore, the developed
biobased UPR nanocomposites are very promising to be applied in structural plastics [3].
Functional fabrics have gained attention as an environmentally-friendly synthesis
route. Yang et al. developed novel bamboo pulp fabrics with thermal conductivity proper-
ties by coating the fabric with graphene and cellulose nanocrystal (G/CNC) solutions. The
influences of G and CNC concentrations on the properties of fabrics were studied. It was
found that the viscosities of the G/CNC solutions increased with an increase of G contents.
G had an obvious thickening effect. Furthermore, compounded fabrics with different G
and CNC contents (GCBPFs) were prepared and extensively characterized in terms of their
thermal and mechanical properties as well as morphology. The ultimate thermal conduc-
tivity, bursting strength, and tensile strength of the GCBPF were 0.136 W/m K, 1.514 MPa,
and 25.8 MPa, with 4 wt.% CNC and 3 wt.% G contents. The results demonstrated that the
as-fabricated GCBPFs with favorable thermal conductivity could be applied as a novel fast
cooling textile for the clothing industry [4].
Under the current situation of frequent oil spills, the development of green and
recyclable high-efficiency oil-absorbing aerogel materials has attracted wide attention from
researchers. Zhou et al. reported a high-strength, three-dimensional hydrophobic cellulose
nanofiber (CNF)/polyvinyl alcohol (PVA)/graphene oxide (GO) composite aerogel with an
anisotropic porous structure, which was fabricated by directional freeze-drying technology
using anisotropically grown ice crystals as a template, followed by hydrophobic treatment
with a simple dip-coating process. The prepared composite aerogel presented anisotropic
multi-level pore microstructures, low density (17.95 mg/cm3 ), high porosity (98.8 %),
good hydrophobicity (water contact angle of 142◦ ), and great adsorption capacity (oil
absorption reaching 96 times its own weight). More importantly, the oriented aerogel had
high strength, whose compressive stress at 80% strain reached 0.22 MPa, and could bear
more than 22 times its own weight without deformation. Therefore, a CNF/PVA/GO
composite aerogel could be prepared by a simple and easy-to-operate directional freeze-
drying method, being a promising absorbent for oil-water separation [5].
Besides the graphene-based materials intrinsic properties and the interactions with
the polymer matrix, the amounts of filler used and the composite production methods
can have an impact on its final properties. Huang et al. studied the effects of increasing
graphene nanosheet (GNS) concentrations on variations in the structure and properties
of electrospun GNS-filled poly(trimethylene terephthalate) (PTT/GNS) composite fibers,
such as in its morphology, crystallization behavior, mechanical properties, and electrical
conductivity. The effects of GNS addition on solution rheology and conductivity were
also investigated. GNSs were embedded in the fibers and formed protrusions. The PTT
cold crystallization rate of PTT/GNS composite fibers increased with the gradual addition
of GNSs. A PTT mesomorphic phase was formed during electrospinning, and GNS
could induce the PTT mesomorphic phase significantly during PTT/GNS composite fiber
electrospinning. The PTT/GNS composite fiber mats (CFMs) became ductile with the

2
Polymers 2021, 13, 685

addition of GNS. The elastic recoveries of the PTT/GNS CFMs with 170 ◦ C annealing were
better than those of the as-spun PTT/GNS CFMs. Percolation scaling laws were applied to
the magnitude of conductivity to reveal the percolation network of electrospun PTT/GNS
CFMs. The electrical conductivity mechanism of the PTT/GNS CFMs differed from that
of PTT/GNS composite films. Results showed that the porous structure of the PTT CFMs
influenced the performance of the mats in terms of electrical conductivity [6]. Hendrix
et al. developed a method exploiting high-speed elongational flow in a novel designed
batch mixer, creating a distribution of pristine few to many layer graphene flakes. The
method focuses on exfoliating in a molten polyamide 66 (PA66) matrix, creating a graphene
reinforced polymer matrix composite (G-PMC). The process revealed that high-speed
elongational flow was able to create few layer graphene. Graphite exfoliation was found
driven in part by diffusion, leading to the intercalation of PA66 in graphite. The intercalated
structure lead to increases in the hydrogen bonding domain, creating anisotropic crystal
domains. The thermal stability of the G-PMC was found to be dependent on the degree of
exfoliation, the PA66 crystal structure, and composite morphology. The aim of this research
was to characterize uniquely produced graphene containing polymer matrix composites
using a newly created elongational flow field. Using elongational flow, graphite can be
directly exfoliated into graphene within a molten polymer [7].
Graphene impermeability against water, oxygen, and ions diffusion, together with its
large surface area, make it an outstanding material for application in anticorrosion surface
coatings. Lei et al. studied the corrosion behavior of zinc-rich epoxy primers or paints
(ZRPs) with different conducting polyaniline-grafted graphene (PANI/Gr) contents. The
conductivity of the formed PANI/Gr nanosheets was significantly improved by employing
Gr as the inner template to synthesize the PANI. The protective properties and the elec-
trochemical behavior of coatings with artificial defects were investigated by monitoring
the free corrosion potential versus time and by using localized electrochemical impedance
spectroscopy (LEIS). A synergetic enhancement of the physical barrier role of the coating
and the zinc sacrificial cathodic protection was achieved in the case of ZRP including
PANI/Gr nanosheets. In addition, the ZRP mixed with the PANI/Gr at a content of 0.6%
exhibited the best anticorrosion performance across the range of investigated PANI/Gr
contents [8].
Graphene and graphene polymer composites have been widely explored for the de-
velopment of medical implants, antibacterial materials, biosensors, drug and gene delivery
systems, as well as phototherapy platforms. Gurunathan et al. produced graphene oxide–
green platinum nanoparticles (GO-PtNPs) using vanillin and studied its effect on human
prostate cancer cells (LNCaP). GO-PtNP cytotoxicity in LNCaP cells was demonstrated by
measuring cell viability and proliferation. Both decreased in a dose-dependent manner
compared to that by GO or PtNPs alone. GO-PtNP cytotoxicity was confirmed by increased
lactate dehydrogenase release and membrane integrity loss. Oxidative stress induced
by GO-PtNPs increased malondialdehyde, nitric oxide, and protein carbonyl contents.
The effective reactive oxygen species generation impaired the cellular redox balance and
eventually impaired mitochondria by decreasing the membrane potential and ATP level.
The cytotoxicity to LNCaP cells was correlated with increased expression of proapoptotic
genes (p53, p21, Bax, Bak, caspase 9, and caspase 3) and decreased levels of antiapop-
totic genes (Bcl2 and Bcl-xl). Activation of the key regulators p53 and p21 inhibited the
cyclin-dependent kinases Cdk2 and Cdk4, suggesting that p53 and p21 activation in GO-
PtNP-treated cells caused genotoxic stress and apoptosis. The increased expression of genes
involved in cell cycle arrest and DNA damage and repair as well as the increased levels
of 8-oxo-deoxyguanosine and 8-oxoguanine suggested that GO-PtNPs potentially induce
oxidative damage to DNA. Thus, GO-PtNPs are both cytotoxic and genotoxic. LNCaP cells
appear to be more susceptible to GO-PtNPs than to GO or PtNPs. Thus, GO-PtNPs have
potential as an alternate and effective cancer therapeutic agent. In other words, this work
shows that the combination of graphene oxide with platinum nanoparticles opens up new
perspectives in cancer therapy. However, further detailed mechanistic studies are required

3
Polymers 2021, 13, 685

to elucidate the molecular mechanism of GO-PtNPs induced cytotoxicity in prostate can-

cer [9]. Costa-Almeida et al. used a one-step thermal reduction and noncovalent chemical
functionalization process to produce PEGylated reduced nanographene oxide (rGOn-PEG)
from nanographene oxide (GOn). Nanomaterials were characterized in terms of particle
size, dispersion stability, chemistry, and photothermal properties, in view of its use for
photothermal therapy (PTT) of nonmelanoma skin cancer. GOn infrared spectrum pre-
sented more intense bands assigned to oxygen containing functional groups than observed
for rGOn-PEG. GOn C/O ratio decreased more than 50% comparing with rGOn-PEG
and nitrogen was present in the latter (N at.% = 20.6) due to introduction of PEG-NH2 .
Thermogravimetric analysis allowed for estimating the amount of PEG in rGOn-PEG to be
of about 56.1%. Simultaneous reduction and PEGylation increased the lateral dimensions
from 287 ± 139 nm to 521 ± 397 nm, as observed by transmission electron microscopy
and dynamic light scattering. It was found that rGOn-PEG exhibited roughly 13-fold
higher absorbance in the near-infrared radiation (NIR) region, as compared to unmodified
GOn. Low power (150 mW cm−2 ) NIR irradiation using LEDs resulted in rGOn-PEG
heating up to 47 ◦ C, which is within the mild PTT temperature range. PEGylation strongly
enhanced the dispersibility of rGOn in physiological media (phosphate buffered saline,
fetal bovine serum, and cell culture medium) and also improved the biocompatibility of
rGOn-PEG, in comparison to GOn (25–250 µg mL−1 ). After a single NIR LED irradiation
treatment of 30 min, a decrease of ≈38% in A-431 cells viability was observed for rGOn-PEG
(250 µg mL−1 ). Together, these results demonstrate the potential of irradiating rGOn-PEG
using lower energy, cheaper, smaller, and safer LEDs as an alternative to high-power lasers
for NIR mild hyperthermia therapy of cancer, namely nonmelanoma skin cancer [10].

Data Availability Statement: No new data were created or analyzed in this study. Data sharing is
not applicable to this article.
Acknowledgments: The editors are thankful for the support from FEDER funds through the COM-
PETE 2020 Operational Programme for Competitiveness and Internationalisation (POCI), Portugal
2020, and by national funds (PIDDAC) through FCT/MCTES in the framework of the project POCI-01-
0145-FEDER-031143, and Base Funding-UIDB/00511/2020 of the Laboratory for Process Engineering,
Environment, Biotechnology and Energy (LEPABE). Artur Pinto thanks the Portuguese Foundation
for Science and Technology (FCT) for the financial support of his work contract through the Scientific
Employment Stimulus-Individual Call [CEECIND/03908/2017].
Conflicts of Interest: The authors declare no conflict of interest.

References
1. Irez, A.B.; Bayraktar, E.; Miskioglu, I. Fracture Toughness Analysis of Epoxy-Recycled Rubber-Based Composite Reinforced with
Graphene Nanoplatelets for Structural Applications in Automotive and Aeronautics. Polymers 2020, 12, 448. [CrossRef] [PubMed]
2. Rahimian-Koloor, S.M.; Karimzadeharani, A.; Hamdi, M.; Petrů, M.; Tamin, M.N. Nano-Level Damage Characterization of
Graphene/Polymer Cohesive Interface under Tensile Separation. Polymers 2019, 11, 1435. [CrossRef] [PubMed]
3. Liu, C.; Wang, C.; Tang, J.; Zhang, J.; Shang, Q.; Hu, Y.; Wang, H.; Wu, Q.; Zhou, Y.; Lei, W.; et al. High-Performance Biobased
Unsaturated Polyester Nanocomposites with Very Low Loadings of Graphene. Polymers 2018, 10, 1288. [CrossRef] [PubMed]
4. Yang, F.; Lan, C.; Zhang, H.; Guan, J.; Zhang, F.; Fei, B.; Zhang, J. Study on Graphene/CNC-Coated Bamboo Pulp Fabric
Preparation of Fabrics with Thermal Conductivity. Polymers 2019, 11, 1265. [CrossRef] [PubMed]
5. Zhou, L.; Zhai, S.; Chen, Y.; Xu, Z. Anisotropic Cellulose Nanofibers/Polyvinyl Alcohol/Graphene Aerogels Fabricated by
Directional Freeze-drying as Effective Oil Adsorbents. Polymers 2019, 11, 712. [CrossRef] [PubMed]
6. Huang, C.-L.; Wu, H.-H.; Jeng, Y.-C.; Liang, W.-Z. Electrospun Graphene Nanosheet-Filled Poly(Trimethylene Terephthalate)
Composite Fibers: Effects of the Graphene Nanosheet Content on Morphologies, Electrical Conductivity, Crystallization Behavior,
and Mechanical Properties. Polymers 2019, 11, 164. [CrossRef] [PubMed]
7. Hendrix, J.W.; Szeto, R.; Nosker, T.; Lynch-Branzoi, J.; Emge, T.J. Evaluation of Exfoliated Graphite to Graphene in Polyamide 66
Using Novel High Shear Elongational Flow. Polymers 2018, 10, 1399. [CrossRef] [PubMed]
8. Lei, Y.; Qiu, Z.; Liu, J.; Li, D.; Tan, N.; Liu, T.; Zhang, Y.; Chang, X.; Gu, Y.; Yin, Y. Effect of Conducting Polyaniline/Graphene
Nanosheet Content on the Corrosion Behavior of Zinc-Rich Epoxy Primers in 3.5% NaCl Solution. Polymers 2019, 11, 850.
[CrossRef] [PubMed]

4
Polymers 2021, 13, 685

9. Gurunathan, S.; Jeyaraj, M.; Kang, M.-H.; Kim, J.-H. Graphene Oxide–Platinum Nanoparticle Nanocomposites: A Suitable
Biocompatible Therapeutic Agent for Prostate Cancer. Polymers 2019, 11, 733. [CrossRef] [PubMed]
10. Costa-Almeida, R.; Bogas, D.; Fernandes, J.R.; Timochenco, L.; Silva, F.A.L.S.; Meneses, J.; Gonçalves, I.C.; Magalhães, F.D.; Pinto,
A.M. Near-Infrared Radiation-Based Mild Photohyperthermia Therapy of Non-Melanoma Skin Cancer with PEGylated Reduced
Nanographene Oxide. Polymers 2020, 12, 1840. [CrossRef] [PubMed]

5
 polymers
Article
Fracture Toughness Analysis of Epoxy-Recycled
Rubber-Based Composite Reinforced with Graphene
Nanoplatelets for Structural Applications in
Automotive and Aeronautics
Alaeddin Burak Irez 1, *, Emin Bayraktar 2 and Ibrahim Miskioglu 3
1 LMT—Laboratoire de Mécanique et Technologie, Université Paris-Saclay, ENS Paris-Saclay, CNRS,
94235 Cachan, France
2 School of Mechanical and Manufacturing Engineering, SUPMECA-Paris, 93400 Saint Ouen, France;
[email protected]
3 ME-EM Department, Michigan Technological University, Houghton, MI 49931, USA; [email protected]
* Correspondence: [email protected]

Received: 31 December 2019; Accepted: 10 February 2020; Published: 14 February 2020

Abstract: This study proposes a new design of lightweight and cost-efficient composite materials for
the aeronautic industry utilizing recycled fresh scrap rubber, epoxy resin, and graphene nanoplatelets
(GnPs). After manufacturing the composites, their bending strength and fracture characteristics were
investigated by three-point bending (3PB) tests. Halpin–Tsai homogenization adapted to composites
containing GnPs was used to estimate the moduli of the composites, and satisfactory agreement
with the 3PB test results was observed. In addition, 3PB tests were simulated by finite element
method incorporating the Halpin–Tsai homogenization, and the resulting stress–strain curves were
compared with the experimental results. Mechanical test results showed that the reinforcement with
GnPs generally increased the modulus of elasticity as well as the fracture toughness of these novel
composites. Toughening mechanisms were evaluated by SEM fractography. The typical toughening
mechanisms observed were crack deflection and cavity formation. Considering the advantageous
effects of GnPs on these novel composites and cost efficiency gained by the use of recycled rubber,
these composites have the potential to be used to manufacture various components in the automotive
and aeronautic industries as well as smart building materials in civil engineering applications.

Keywords: toughening mechanisms; graphene nanoplatelets; recycled rubber; Halpin–Tsai; SEM

1. Introduction
Over the past decades, aeronautic companies have been continuously trying to reduce the overall
cost and mass of an aircraft to better compete with their rivals. Mass reduction leads to lower fuel
consumption and CO2 emissions. Therefore, development of low-cost and lightweight materials to
be used in the manufacture of various aircraft parts constitutes an important task for engineers in
aeronautic companies.
In aircrafts, polymer-based composites are used widely in the manufacturing of various structural
and functional components including the wings, tail, and skin panels. In material selection, structural
requirements are, of course, important. Also, the cost of the material should be minimized without
compromising the structural requirements. To that end, proposing a low-cost, lightweight aircraft
material was the main objective of this study.
Polymer-based composites are extensively used to manufacture lightweight structural components.
Including recycled materials in the production may result in cost efficiencies as well as ecological
solutions. Epoxy, a thermosetting polymer, which is relatively easy to process and has low cost, is

Polymers 2020, 12, 448; doi:10.3390/polym12020448 7 www.mdpi.com/journal/polymers

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