Received: 6 July 2023 Revised: 20 September 2023 Accepted: 21 September 2023

DOI: 10.1002/pc.27825

RESEARCH ARTICLE

Influence of surface-treatment of bamboo fiber on the

physico-mechanical properties of bamboo fiber composites
with virgin and recycled high-density polyethylene

Santoshi Mohanta 1,2 | Priyanka Mahalik 1 | Gayatri Prasad Hota 1 |

Bipin Bihari Sahoo 1 | Subhransu Sekhar Pradhan 3 | Shyama Prasad Mohanty 1

1
Central Institute of Petrochemicals
Engineering and Technology: Institute of Abstract
Petrochemicals Technology (CIPET: IPT), Natural fiber-reinforced composites are showing promising results compared
Bhubaneswar, India
to synthetic fiber-reinforced composites. Therefore, the present work high-
2
School of Chemical Technology, Kalinga
lights the utilization of chemically treated bamboo-fiber (BF) for the prepara-
Institute of Industrial Technology,
Bhubaneswar, India tion of bamboo-fiber high-density polyethylene composites (BF/HDPE). Both
3
Laboratory for Advanced Research in virgin HDPE and recycled HDPE (r-HDPE) are considered for the preparation
Polymeric Materials (LARPM), Central of bamboo fiber (BF) composite and their physico-mechanical properties are
Institute of Petrochemicals Engineering
and Technology (CIPET), evaluated. On alkali and stearic acid treatment, more fibrillation and surface
Bhubaneswar, India roughness are observed in the BF surface which created more contacting sur-
faces to improve the interfacial interaction between the BF and HDPE &
Correspondence
Shyama Prasad Mohanty, Central r-HDPE matrix. The tensile strength of stearic acid-treated BF/HDPE is
Institute of Petrochemicals Engineering increased by 9.26% and stearic acid-treated BF- rHDPE shows an increment of
and Technology: Institute of
16.5%. Similar observations are made for impact strength which confirms the
Petrochemicals Technology (CIPET: IPT),
B-25, C.N.I. Complex, Patia, Bhubaneswar improved dispersion of BF in both matrices. The improved interfacial bonding
751024, Odisha, India. between BFs and HDPE matrix and good dispersion between fibers and matrix
Email: [email protected]
can further be confirmed through the SEM images of composite fractured sur-
faces and FTIR analysis.
Highlights
• Surface of BF has been modified by NaOH and stearic acid treatment.
• Modified fibers are used as reinforcement in virgin and r-HDPE composites.
• Stearic acid treatment enhances the tensile strength of composites.
• Surface modification has significant impact on r-HDPE composites.

KEYWORDS
bamboo fiber, HDPE, mechanical property, natural fiber composites, stearic acid treatment

1 | INTRODUCTION weight compared to glass fibers, environmental advan-

tages, and many more. Natural fibers can be extracted
Natural fibers are nowadays favored over synthetic fibers from several parts of plants and are classified accordingly:
as a reinforcement material in polymeric composites bast fibers (jute, flax, hemp, kenaf, etc.), leaf fibers (sisal,
because of their numerous advantages such as abundance palm, curaua, etc.), stalk fiber (bamboo, sugarcane, rice,
availability, non-toxic, high performance, low cost, light etc.), seed fibers (cotton, kapok, etc.), and fruit fiber

914 © 2023 Society of Plastics Engineers. wileyonlinelibrary.com/journal/pc Polymer Composites. 2024;45:914–923.

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MOHANTA ET AL. 915

(coconut, coir, etc.).1 These fibers are used as reinforce- the NFRCs. Therefore, various treatments are performed
ment for polymer composites and result in natural on the BFs like heat treatment, high-energy irradiation,16,17
fiber-reinforced composite (NFRCs/NFCs). NFRCs are chemical and biological treatments,15,18 use of compatibili-
environmentally attractive materials that are proven to zers and coating19 and many more to modify the surface.
be an alternative to the conventional glass fiber or carbon All these approaches are performed eventually to improve
fiber-reinforced composites (GFRCs or CFRCs). As the adhesion property of fibers with the matrix in the com-
reported, the major increase in demand for NFCs is posite. It has been reported that natural fibers are treated
mainly because of their huge demand in automotive and with different chemicals such as alkaline, silane peroxide,
construction applications.2 Moreover, these NFRCs are and permanganates.18 On chemical treatment, some com-
widely used in low-cost housing, civil structures, con- ponents of these fibers get detached from the fiber struc-
sumer goods, and many other applications.1 ture or the crystalline structure might change which
Among the available NFRCs, the usage of bamboo ultimately improves the mechanical, thermal and other
fibers composites (BFCs) has gained attention nowadays. properties. Several studies have reported a reduction in
This is mainly because of high mechanical properties, dampness/swelling of natural fibers by chemical treat-
environmental sustainability, and competitive perfor- ment.10 Chemical treatment with appropriate reagents has
mance with those of glass fibers.3 Additionally, bamboo further improved the mechanical strength of BFCs. This
fibers (BFs) show excellent flexibility as a reinforcement shows the chemical treatment enhances the interfacial
material that can be used in various forms, like strands,4 bonding between BF and the polymer matrix. Surface mod-
fibers,5,6 bamboo charcoal,7 and flour.8 It has been ification of fibers occurs during chemical treatment. Zhang
reported in several studies that short BFs have been uti- et al.20 investigated the effect of sodium hydroxide treat-
lized to improve the mechanical and thermal properties of ment on the microstructural, thermal and mechanical
high-density polyethylene (HDPE) composites.9–11 BFs are properties of BFs. Due to alkali treatment, surface area of
also found to perform better compared to bamboo flour. fibers was increased as compared to untreated fibers. This
Similarly, the incorporation of bamboo charcoal shows sig- resulted in enhancement in thermal stability and tensile
nificant improvement in the mechanical and electrical strength of the BFs.
properties of ultra-high molecular weight polyethylene As reported in the previous studies, the BFCs are
composites.12 Yang et al.13 have prepared unidirectional mainly prepared with virgin thermoplastic matrix which
BF-epoxy composites and observed significant improve- includes HDPE, polypropylene (PP), polyvinyl chloride
ment in the mechanical properties and thermal stability of (PVC), and many more.21–23 However, very limited works
the composites. Glass transition temperature (Tg) have been reported on recycled thermoplastic based BFCs
decreased whereas thermal stability increased in the com- or NFCs. Moreover, with the raising concern over the
posites due to the presence of BFs. Significant improve- global energy crisis and environmental pollution due to
ment in tensile strength and modulus of composites was petroleum-based thermoplastic wastes, there is a growing
observed due to the reinforcing effect of the fibers. demand in the effective utilization of virgin thermoplas-
Recently, Shi et al.14 investigated the effect of BF preform tics. It is well-known that post-consumer thermoplastic
on the mechanical and thermal properties of BF-epoxy materials generated each year contribute around 10% of
composites. The incorporation of BFs into epoxy signifi- solid municipal waste.24 Therefore, efforts have been made
cantly improved the flexural, shear and impact properties, in recycling and reuse these thermoplastics and hence,
thermal properties and interface properties of the epoxy increasing their service life. So, it is important to explore
resin. In another work, Wang et al.15 investigated the the possibility of using recycled HDPE (r-HDPE) as raw
effect of BF volume fraction on the mechanical and ther- material for NFCs to attain environmental sustainability.
mal properties of PLA-BF composites. They reported sig- Therefore, in the present work, the mechanical and
nificant improvement in tensile modulus and strength thermo-physical properties of composites prepared with
with increase in fiber content. Additionally, with the incre- virgin HDPE (BF-vHDPE) and rHDPE (BF-rHDPE) is
ment of fiber content Tg and crystallization temperature systematically studied. The effects of surface treatment of
(Tc) of composites also increased. BFs on the properties of BF-vHDPE and BF-rHDPE are
These BFs are showing promising results in the investigated. Scanning electron microscopy (SEM),
improvement of mechanical and thermal properties of vari- Fourier-transform infrared (FTIR) spectroscopic analysis,
ous polymeric composites, however, the interfacial bonding and thermogravimetric analysis (TGA) are used to study
between the fibers and the polymer is still a matter of con- the effect of surface modification on the fibers. Addition-
cern. In general, the natural fibers are highly hydrophilic ally, tensile, impact, and water absorption properties are
thus resulting in reduced adhesion with the polymer further investigated on composites to confirm the appli-
matrix and negatively affecting the overall performance of cability of BF-rHDPE composites.
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916 MOHANTA ET AL.

2 | MATERIALS AND METHODS it and vigorously stirred for 1 h. The resulting mixture
was filtered and washed several times with distilled
2.1 | Materials water. Afterwards, the BFs were kept in an oven at 60
C
for approximately 12 h and labeled as SA-BF.
The matrix materials used in the present study are HDPE
and r-HDPE. The HDPE (Halene-H, Grade-B6401) was
provided by Haldia Petrochemicals Ltd, India. It has a 2.2.3 | BF/HDPE composite preparation
melt flow index (MFI) of 0.4 g/10 min (2.16 kg, 190
C),
melting point of 132
C, and a density of 0.964 g cm3 as Several BF/HDPE composites were prepared using the
provided by the manufacturer. The r-HDPE was collected melt-blending technique. At first, the BFs were oven
from a plastic manufacturing lab of Bhubaneswar, dried at 60
C and the composites were manufactured by
Odisha, India. MFI of r-HDPE was found to be melt-blending of treated BFs and HDPE/ r-HDPE in a
18.05 g/10 min. BFs used in this study were extracted high-speed twin screw extruder at a mass ratio of 3:7.
from Petung bamboo also known as Dendrocalamus Asper The barrel temperatures were maintained at
which is about 3 and 4 years old. The bamboo culm was 180/190/205/210
C and the screw speed was maintained
collected from Odisha, India. Sodium hydroxide (Extra at 90–100 rpm. The polymer melt from the twin-screw
Pure, Research Lab Fine Chem Industries, India) and extruder went directly through the die at the end of the
stearic acid (Synthesis grade, Labogens, India) were used nozzle, cooled down to room temperature and then
for the surface treatment of fibers. chopped into small granules. The granules formed were
further dried in an oven and were injection molded as
per ASTM standard using SP130 injection molding
2.2 | Methods machine (Windsor, India) having clamping force 130 T.
The composite samples prepared are labeled and pro-
2.2.1 | BP extraction vided in Table 1.

The BFs were extracted mechanically. In this method,

the bamboo culm was initially cut into smaller strips 2.2.4 | Tensile test
from the middle section, and the top skin was removed.
The strips were further soaked in water for 1 h to facili- To understand the effect of various chemical treatments
tate the separation of fibers from the strips. The soaked on BFs, mechanical properties of the prepared BF-
strips were then passed through a two-roll mill (Neoplast HDPE composites were evaluated. The mechanical
Engineering (P) Ltd., Ahmedabad, India) operating at a strength was estimated by performing tensile and
lower speed under slight pressure and crushed BF was impact tests. For tensile test, five test specimens were
collected. The crushed BF strips were dried in an oven cut according to ASTM D 638 standards. Dog-bone spec-
for 12 h maintained at 60
C. These dried BFs are further imens with dimensions of 165 mm  13 mm  3 mm
crushed in a crusher and approximately five mesh-size were prepared. A universal testing machine (UTM),
BF samples are prepared. Instron 3382, UK is used for tensile strength tests. In
this study, the tensile tests were carried out at a cross-
head speed of 50 mm/min.
2.2.2 | Chemical treatment of BF

The crushed BFs were further undergone alkali treat- 2.2.5 | Impact test
ment by soaking in 5 wt% NaOH solution for 1 h to
reduce the chemical content of the BFs as per previous I-zod impact test specimens having dimensions of
published literature studies.11,25,26 The alkali treated BFs 63.5 mm  12.7 mm  3.2 mm were prepared. Five
were washed with distilled water until neutral pH was V-notched samples having a notch depth of 2.54 mm and
obtained. These were further dried in an oven at 60
C for an angle of 45
were prepared and tested according to the
approximately 12 h and labeled as SH-BF. ASTM D 256-05 using Izod impact tester (Impact-104,
Another set of BFs was treated with stearic acid Tinius Olsen, USA). All specimens were stored under
followed by NaOH treatment. To prepare stearic acid controlled environment conditions and at least five sam-
solution, 30 g of stearic acid was added to 1000 mL of ples were tested for each measurement. Standard devia-
ethyl alcohol. The mixture was heated until the stearic tions are calculated accordingly, and each plot are shown
acid was completely dissolved. The SH-BF was added to with error bars.
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MOHANTA ET AL. 917

T A B L E 1 Composition of samples prepared by compounding 2.2.9 | Thermal gravimetric analysis

treated BFs and polymer.

Constituents of BF/
TGA was conducted using a TGA 8000, PerkinElmer,
HDPE composite Label USA equipment to study the thermal degradation behav-
ior of the chemically treated BFs. All samples were
HDPE V
heated in an inert atmosphere on platinum pans. Approx-
SH-BF/HDPE V+
imately, 10 mg of all samples were taken and heated from
SA-BF/HDPE V++ ambient temperature to 700
C at a heating rate of 10
C/
r-HDPE R min under N2 atmosphere.
SH-BF/r-HDPE R+
SA-BF/r-HDPE R++
2.3 | FTIR Analysis

2.2.6 | Water absorption test FTIR spectroscopy of chemically treated (SH-BF and
SA-BF) and untreated BF (U-BF) were conducted in a
For the water absorption test, the specimens were first Spectrum two PerkinElmer instrument. The analysis was
dried in an oven for 24 h at 60
C and then placed in conducted in the mid infrared range of 400–4000 cm1 at
desiccators to cool down to room temperature. Imme- a resolution of 4 cm1 in attenuated total reflectance
diately upon cooling the specimens were weighed. The (ATR) mode.
specimens were then immersed in water at 23 ± 2
C
for 24 h. Specimens were removed, patted dry with a
lint free cloth, and weighed. For each measurement 3 | RESULTS A ND DISCUSSION
three specimens were taken, and the average weight
was considered. The water absorption study was 3.1 | Effect of chemical treatment on
conducted for 72 h and the results are analyzed. The fiber morphology
percentage water absorption is calculated as per
Equation (1). The surfaces of the BFs used in the present study are
chemically treated to improve the fiber–matrix interfacial
Percent water absorption ¼ bonding and to reduce the hydrophilicity of BFs. These are
undergone alkali treatment (NaOH) and stearic acid fol-
Weight of wet sample  Initial weight of dry sample
 100: lowed by alkali treatment, respectively. The surface mor-
Initial weight of dry sample
phology of alkali treated (SH-BF) and alkali and stearic
ð1Þ acid treated BF (SA-BF) are shown in Figure 1A, B. The
surface of SH-BF appears to be quite rough with fibrils
2.2.7 | SEM Analysis growing over the surface. This is probably due to the
removal of the surface materials consisting of hemicellu-
The morphology of chemically treated BF and the impact loses, lignin, wax, and impurities on application of NaOH.
fractured surface of BF-HDPE composite are analyzed by Treatment with NaOH is known to enhance the surface
SEM model no. JEOL JSM-6610. All samples are sput- area of fibers.20 The surface roughness may find to be ben-
tered with a thin layer of gold before SEM observation. eficial for promoting the mechanical interaction between
BF and the polymer matrix which further improve the
adhesion property. The SEM images of SA-BF samples as
2.2.8 | Differential scanning calorimetry shown in Figure 1C, D. It can be observed that the surface
analysis of the fibers appears to be smooth as compared to SH-BF.
Treatment of fibers with stearic acid results in smooth sur-
The thermal properties of chemically treated r-HDPE- face due to coating of stearic acid as a layer on the fibers.
BF composites (R, R+, and R++) are evaluated by
performing differential scanning calorimetry (DSC)
analysis using a Diamond DSC, PerkinElmer, USA at a 3.2 | FTIR analysis of chemically
heating rate of 10
C/min. For each analysis a sample of modified BFs
≤5 mg was weighed and sealed. All scans were per-
formed at a temperature range of 35-200
C under N2 The chemically treated BFs are characterized by
atmosphere. FTIR analysis. The plot of FTIR spectra of untreated
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918 MOHANTA ET AL.

FIGURE 1 SEM micro-graphs of SH-BF (A, B) and SA-BF (C, D) at different magnifications.

BF (U-BF), NaOH-treated BF (SH-BF) and NaOH-

stearic acid-treated BF (SA-BF) are shown in
Figure 2.
BFs are mainly composed of cellulose, hemi-
cellulose, and lignin. All these components are iden-
tified from the FTIR spectra of U-BF. The peak at
3419 cm1 is mainly attributed to the –OH stretching
vibration of hydroxyl groups while at 2936 cm1 is
assigned to C H asymmetric stretching. For alkaline
treated BF (SH-BF) the peak around 1745 cm1
disappears, this is assigned to the ester groups in
hemi-cellulose of BFs. This confirms the degradation
of hemi-cellulose and lignin on the BF surface.
Similar observations are also made for SA-BF
spectra. Additionally, the peak intensity between
2936 and 2849 cm1 increased in SA-BF spectra
which correspond to C H asymmetric stretching FIGURE 2 FTIR spectra of U-BF, SH-BF, and SA-BF
vibration. samples.
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MOHANTA ET AL. 919

3.3 | Thermal analysis of the could be mainly resulted due to the decomposition of cel-
modified BFs lulose and hemicellulose. With the increase in tempera-
ture, the degradation product was converted into water
The plots obtained from thermogravimetric analyses for and carbon dioxide in presence of excess oxygen. The
SH-BF and SA-BF are presented in Figure 3. It can be degradation of hemicellulose is observed at around 290
C
seen from Figure 3, the TGA curve of chemically treated for untreated BF.27 However, after alkali treatment, this
BF show the weight loss at various temperature regimes. peak was almost vanished, confirming the complete
In between 30
C and 150
C, the initial weight loss removal of hemicelluloses from BF. These TGA results
occurred which may be the result of evaporation of implied that surface treatment of BF helped in improving
absorbed moisture present in the BF fibers as reported by the thermal stability and reduction in the surface
Wang et al.27 After surface modification with alkali and hydrophilicity.
acid treatment, the weight loss becomes significantly less
than that of U-BF below 150
C. This shows that the
water adsorption was reduced by attachment of hydro- 3.4 | Tensile test
phobic groups to the BF. Additionally, the occurrence of
multi-stage weight losses shown from 250
C to 350
C The physical and mechanical properties of virgin HDPE
(V), r-HDPE (R) and different BF/HDPE composites such
as the chemical treated specimens (V+, V++, R+, and R+
+
) are shown in Figure 4. The tensile strength and yield
strength are plotted in Figure 4A and B, respectively. It
can be noted from these plots that, the BF/HDPE com-
posites (V++) prepared after chemical treatment of the
fibers show improved tensile properties compared to
the unreinforced specimen (V). Stearic acid treated
BF/HDPE (V++) composites show an enhancement of
tensile strength by 9.26%. Similarly, the BF/r-HDPE com-
posites (R) show an enhancement in tensile strength with
chemical treatment and the R++ composites show an
increment of 16.5%. On chemical treatment, there was a
rupture in ester linkage between poly-uronic acid and lig-
nin which increases crystalline index. Accordingly, the
fibers become less dense and more rigid which gives bet-
ter tensile property. The results are in accordance with
FIGURE 3 TGA plot of SH-BF and SA-BF samples. the published literature.25 The yield strength is found to

FIGURE 4 Tensile strength (A) and Yield strength (B) of V, V+, V++, R, R+ and R++ specimens.
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920 MOHANTA ET AL.

FIGURE 5 Impact strength of V, V+, V++, R, R+, and R++ FIGURE 6 The water absorption of V, V+, V++, R, R+, and R+
specimens. +
specimens.

be decreasing with chemical treatment for all the

composites. responsible for formation of hydrogen bond with water
molecules. So, the overall water absorption of the
BF-HDPE composites depends on the available free
3.5 | Impact test hydroxyl groups. In Figure 6, the water absorption per-
centage of all the specimens prepared such as V, V+,
The impact strength of fiber-reinforced composites V++, R, R+, and R++ are presented which clearly
depends on the fiber–matrix interfacial bonding, fiber ori- shows the effect of alkali and stearic acid treatment on
entation and the percentage of fiber present. To under- the BFs. The water absorption of HDPE (V) shows
stand the effect of chemical treatment on the overall 1.00% after 72 h of water immersion. However, with
impact strength of the prepared HDPE-BF composites alkaline and acid treatment the water absorption percent-
I-zod impact test was conducted. The results of HDPE age decreases to 0.53% and 0.27% for NaOH-treated and
(V), r-HDPE (R) and the chemical treated specimens (V+, stearic acid treated BF/HDPE composites (V+, V++),
V++, R+, and R++) are shown in Figure 5. For BF/HDPE respectively. This is because the alkaline treatment reduces
composites the surface treatment of BFs by NaOH shows the content of hemi-cellulose and lignin in BF which in-
improvement in impact strength but V++ samples does turn increases its hydrophobicity. Similarly, on further
not show any such improvement. However, for BF/r- treatment with stearic acid shows more hydrophobic
HDPE composites significant improvement in impact behavior and water absorption percentage reduces further.
strength is observed in alkali and acid treated BF/r-HDPE The water absorption of the BF/rHDPE composites is
composite samples. The chemical treatment led to an lower compared to their virgin counter parts. The R++
increase in 30% and 39% I-zod impact strength compared composites show least percent of water absorption which
to the unreinforced one. The r-HDPE composites rein- is around 0.021%.28
forced with chemically treated BF shows good adhesion
between polymer and fibers which increased in impact
strength. 3.7 | DSC Analysis

The thermal behavior of r-HDPE and chemically trea-

3.6 | Water Absorption Test ted r-HDPE-BF composites (R, R+ and R++) are evalu-
ated by performing DSC analysis. The plots for heating
In BF/HDPE composites, moisture is absorbed mainly and cooling cycles are presented in Figure 7A, B,
by the BFs which are hydrophilic in nature. The free respectively.
hydroxyl groups of cellulose, hemi-cellulose and lignin It can be observed from the Figure 7A that, with
present abundantly on the surface of BFs are mainly incorporation of chemically treated BF, the melting
 15480569, 2024, 1, Downloaded from https://4spepublications.onlinelibrary.wiley.com/doi/10.1002/pc.27825 by Malaviya National Institute of, Wiley Online Library on [06/04/2025]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License
MOHANTA ET AL. 921

FIGURE 7 DSC plots for heating (A) and cooling (B) cycles of R, R+, and R++ specimens.

FIGURE 8 SEM micro-graphs of SH-BF/HDPE (A–C) and SA-BF/HDPE (D–F) composites fractured surface at different magnifications.

point of r-HDPE has reduced from 164.2
C to 146.4
C. 3.8 | SEM observation of composites
This significant reduction in melting point confirms the fracture surface
presence of genuine interface between the BF and
r-HDPE matrix.9 The interaction between fibers and The morphology of fractured BF composite samples is
matrix is attributed by the presence of stearic acid at the further analyzed by SEM as shown in Figure 8, which
interface. The peak crystallization temperature (Tc) was reveals the presence of fiber breakage, fiber pull out from
reported from the first cooling cycle as shown in Figure 7 the matrix and well dispersion of BF in the matrix.
(b). For r-HDPE no peak is observed and for treated Figure 8B shows BF surfaces are covered by the HDPE
r-HDPE-BF composites little difference in Tc is found. matrix confirming good fiber–matrix bonding. The
 15480569, 2024, 1, Downloaded from https://4spepublications.onlinelibrary.wiley.com/doi/10.1002/pc.27825 by Malaviya National Institute of, Wiley Online Library on [06/04/2025]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License
922 MOHANTA ET AL.

surface treatment of BFs increased surface roughness for ORCID

improved mechanical attachment of the matrix. Eventu- Subhransu Sekhar Pradhan https://orcid.org/0000-
ally produces smoother surface and make oxygen func- 0002-2153-9043
tional groups available for chemical reactions which Shyama Prasad Mohanty https://orcid.org/0000-0001-
results in improved interfacial bonding. 8488-156X
Similarly, Figure 8F shows considerable amount of
HDPE is attached on the BF surfaces, which indicates RE FER EN CES
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CONFLICT OF INTEREST STATEMENT
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The authors declare that there is no conflict of interest. 14. Shi J, Zhang W, Zhang J, Yuan S, Chen H. Mechanical, ther-
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