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Tube-like natural halloysite/poly(tetrafluoroethylene) nanocomposites: simultaneous

enhancement in thermal and mechanical properties

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2017 Mater. Res. Express 4 045301

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Mater. Res. Express 4 (2017) 045301 https://doi.org/10.1088/2053-1591/aa68b6

PAPER

Tube-like natural halloysite/poly(tetrafluoroethylene)


nanocomposites: simultaneous enhancement in thermal
RECEIVED
25 January 2017

and mechanical properties


RE VISED
22 March 2017
ACCEP TED FOR PUBLICATION
23 March 2017
PUBLISHED
SureshGamini1, VVasu1 and SuryasarathiBose2
1
10 April 2017 Department of Mechanical Engineering, National Institute of Technology, Warangal, Telangana, 506004, India
2
Department of Materials Engineering, Indian Institute of Science, Bangalore, 560012, India
E-mail: sbose@materials.iisc.ernet.in

Keywords: PTFE, HNTs, storage modulus, tensile modulus, hardness

Abstract
In the current study, PTFE (polytetrafluroethylene) matrix is reinforced with different wt%
(2%10%) of Halloysite nanotubes (HNTs). PTFE samples are fabricated with 2 wt% increment
and are designated from Bto F and designation A refers to neat PTFE. Thermal and mechanical
characterization of the fabricated composites is studied. The calorimetric measurements showed
enhanced degree of crystallinity of the nanocomposites, which is from 57.83% to 74.7%. The
dynamic mechanical analysis results have shown enhanced storage modulus and loss modulus and
reduced damping behaviour, without affecting glass transition temperature. Moreover, significant
improvements in mechanical properties are observed from the experimental results. The results are
discussed and validated with the existing literature. The phase and the fracture morphology of the
nanocomposites is studied using scanning electron microscope and discussed herein.

Introduction

PTFE (polytetrafluoroethylene) is an excellent solid lubricant material preferred as sliding bearing in mechanical
systems such as automotive, textile, food machinery, and in various medical equipment [1]. Although, PTFE
shows excellent self-lubrication characteristics, it has inferior functional properties like low elastic modulus, low
wear resistance, low storage modulus, low degree of crystallinity etc. PTFE is a linear chain polymer consisting of
repeating smooth profile of tetrafluoroethylene (C2F4) units [2]. The fluorine encasement of the carbon backbone
provides high chemical inertness and high working temperature range, whereas, the smooth profile provides low
coefficient of friction. The presence of fluorine content weakens mechanical and thermal properties. The low
degree of crystallinity and heat capacity increases the wear rate and decreases the life cycle of PTFE components.
The degree of crystallinity is associated with functional performance of any polymer composites. Hence, along
with thermal properties, improved mechanical performance is also essential. The work reported by Blanchet and
Kennedy [3], and Makinson and Tabor [4] depicted that the progressive delamination wear process causes severe
wear of PTFE at high speeds and operating temperatures. This has precluded its use as pristine PTFE in many
applications and motivates the use of reinforcement to overcome the onset of severe wear.
Collective researches showed that the addition of low amount of organic and inorganic nanofillers can render
superior improvement of functional properties. In this regard carbonaceous nanoparticles such as graphene sheets
(GS) and carbon nanotubes (CNTs) have gained great deal of interest as a functional filler for polymer-based nano-
composites. In recent study, Graphene nano platelets (GNPs) was used as reinforcement in polydimethylsiloxane
(PDMS) silicone elastomers and the effect of concentration of GNPs on ultimate properties of composites was
studied [5]. From the study, useful mechanical and thermal properties were analyzed through Infrared mechanical
responses at different pre-strain values. The improved properties of the composites have witnessed several varie-
ties of applications like photo-responsive coating material for many MEMS devices, opto-mechanical memory,
adaptive skin smart material, temperature sensitive strain gauge etc. An optimum increase in mechanical proper-
ties such as Youngs modulus, photomechanical induced stresses in the composite material at different pre-strain
levels was realized at 2 wt% GNPs addition. The addition of graphitic nano-carbons such as single layer graphene

2017 IOP Publishing Ltd


Mater. Res. Express 4 (2017) 045301 S Gamini etal

and graphene nano platelets (SLGs and GNPs) as reinforcement played an important role in enhancing several
mechanical properties through improved load transfer Xu etal [7]. During their preliminary studies, they devel-
oped advanced PDMS composites containing SLGs and GNPs for robotic actuator applications. The remarkable
enhancement in load transfer and mechanical properties was observed for PDMS composites containing 1 wt%
exfoliated graphene and it was ascertained with the help of strain induced Raman band shift. Due to the band
shift in tension and compression modes, a considerable increase in mechanical properties such as elastic modulus
of PDMS (about 42%), toughness (about 39%), damping capability (about 673%), and strain energy density
(about 43%) was reported. It was also observed that the orientation of the GNP and SLG flakes in PDMS matrix
influences the damping and frictional properties in longitudinal and transverse loading [6]. The synergistic effect
of multi-wall carbon nanotubes (MWNTs) and SLGs towards load transfer and enhanced mechanical properties
was studied in PDMS matrix. The significant improvement in the load transfer as well as mechanical properties
was obtained with total 1 wt% addition of MWNTs and SLGs in the matrix material [7]. The extensive studies by
Burris etal [810] showed a prominent improvement in mechanical and wear properties for PTFE composites
with organic and inorganic nanofillers compared to micron sized fillers due to its large aspect ratio. Conte etal
[11] has observed that combination of soft and hard phases influenced the coefficient of friction, self-lubricating
and load carrying properties of PTFE composites as compared to pure PTFE. The studies by Feng etal [12]
showed an enhanced tribo-performance with the dispersion of surface modified ZnO nanoparticles in PTFE
matrix. Improved mechanical, wear and electrical properties were reported in single walled carbon nanotube
(SWNT)/PTFE composites [13]. Optimum performance in tensile properties of GF/PTFE composites was found
at 0.3 wt% of surface modified glass fibers by using rare earth surface modifier (LaCl3) [14].
A survey on the natural mineral Halloysite nanotubes (HNTs) being used as filler for thermoplastic, thermoset,
and elastomer polymers, was reported by Rawtani etal [15]. Halloysite nanotubes have alternate alumino silicate
layers with alumino layers located inside the HNTs and most of outer layers are siloxane. The HNTs are usually
hydrophobic in nature due to low content of hydroxyl groups on their surface compared to other nanoclays and
nanosilica. Therefore, HNTs can be easily dispersed in non-polar polymers like PP, ABS, PTFE etc, using shear mixers
[1618]. Also in case of CNTs, owing to interactions, the dispersion in polymer matrices is complex [19]. On the
other hand, HNTs have very less inter-tube relations due to less hydroxyl groups and also the presence of siloxane
makes the inter-tube interaction relatively weak and promotes exfoliated dispersion in the polymer matrix [16]. In
addition, it possess high aspect ratio and cost effectiveness compared to single or multiwalled carbon nanotubes.
HNTs have emerged in its usability as filler in comparison to other nanofillers for polymer-based nanocomposites.
This is in comparison to the effect of fillers like talc, mica and various other aluminum silicates used to improve
functional properties of several polymers [20, 21]. Consequently, modified HNTs were dispersed in the several
polymer matrices such thermoset/thermoplastic/elastomers [18, 2228] and improved functional properties were
found. Moreover, the recent trend in developing green tribological materials has been motivated in the preparation
of PTFE/HNT nanocomposites as PTFE is recyclable and HNTs are naturally available materials. In the present
context, green tribology means saving energy, improving the environment and the quality of life [29]. The PTFE
nanocomposites containing HNTs are not well established in the literature. Therefore, in this study, we have made an
attempt to design PTFE nanocomposites containing HNTs as a functional fillers and their thermal and mechanical
performance was systematically studied. The remarkable enhancement in the mechanical performance of PTFE
nanocomposites containing HNT was realized over neat PTFE. Hence, this study provides critical insights in the
designing of PTFE nanocomposites containing HNT with enhanced mechanical performance.

Experimental methods

Materials
PTFE powder with average particle size of 25 m and INOFLON 640 wear grade is procured from GFL, Gujarat.
HNTs are procured from NaturalNano Inc., USA. HNTs (Al2[Si2O5(OH)4] 2H2O) are hollow tubular structures
with alternate alumino-silicate layers with inner diameter, outer diameter and length of 20nm, 50nm and 200nm,
respectively [30]. Figures1(a) and (b) shows the SEM images of untreated HNTs.

Fabrication of PTFE nanocomposites sheets


At high temperatures, the melt viscosity of PTFE is very high. Therefore, the processing of PTFE is very difficult
using melt intercalation or injection molding [31]. In order to avoid complexities in processing, compression
molding technique followed by sintering is normally employed.
The PTFE nanocomposite sheets are fabricated in to sheets of 300mm300mm3.2mm size. The sheets
are made with 2 wt%10 wt% with 2 wt% increment and are designated as samples AF. These are fabri-
cated by following the sequence of steps: production of preforms, breathing, sintering, cooling, and cleaning. The
preform is a compacted sheet, which is made by pressing the premixed PTFE powders (ensemble) in the mould.
An operating pressure of 14MPa is applied for about 20min. and later the sheets are ejected out of the mould. A

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Mater. Res. Express 4 (2017) 045301 S Gamini etal

Figure 1. SEM images of HNTs (a) at 10000magnification; (b) a single HNT particle on 100nm scale.

Figure 2. (a) Preform sheet; (b) sintering cycle

typical preform sheet is seen from figure2(a). The preforms are kept for 12h at room temperature as a breathing
period in order to release any entrapped air or moisture. Subsequently, they are sintered in an electrical furnace as
per heating and cooling sintering cycle shown in figure2(b), for 8h of holding time at 365 C. Finally, after diag-
nosing the sheets for defects like sintering cracks, and bending of sheets, the blur edges of each sheet are cleaned by
wiping with a medium grade abrasive paper. Later, the specimens are cut from these sheets for characterization as
per ASTM standards for different tests.

Morphological study
X-ray diffraction analysis (XRD)
The XRD patterns for the nanocomposite are studied using a PANalytical XPert PRO diffractometer. The PTFE
nanocomposites samples are scanned from 10 to 50 and intensity values recorded.

Thermal characterization
Differential scanning calorimetry (DSC)
Differential scanning calorimetry tests are performed using Mettler-Toledo DSC822e, at a heating rate of 5 C
min1 from 40 C to 375 C in nitrogen environment. The heat of fusion (mJ mg1) of the nanocomposites is
estimated by measuring the area of heating peaks. The degree of crystallinity or % cryallinity denoted by % Xc, is
defined as:
Area of the melt endotherm, (Hf )
% Xc = .
Theoritical heat of fusion, (H100f )
For different wt% addition of HNT in the matrix material, the % crystallinity can be estimated by using
equation(1) [32].
Hf
% Xc =
(1) 100
H100f (1 wt )

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Mater. Res. Express 4 (2017) 045301 S Gamini etal

Table 1. XRD parameters of %HNT loading.

Designation Position (2 theta) Intensity (a.u.) d spacing ()

A
B 12.38 1826 7.14
C 12.31 1979 7.18
D 12.31 2182 7.18
E 12.27 2451 7.21
F 12.31 2487 7.18

where, Hf=area of the melt endotherm in J g1; H100f=heat of fusion for a 100% crystalline PTFE sample;
wt=wt% of HNT, see table1.

Dynamic mechanical analysis (DMA)


The visco-elastic behavior of the PTFE composites is studied by a dynamic mechanical analyser. The measurements
are done on a single cantilever test clamp. The samples are deformed periodically at a frequency of 1 Hz over a
varying temperature from 30 C to 200 C with oscillation amplitude of 15 m. The variation in the storage
modulus (E, which is the measure of elastically stored energy), loss modulus (E) and the tangent of the phase
angle (tan=E/E) have been analyzed as a function of temperature.

Mechanical characterization
Tensile properties
The tensile tests are carried out on Instron make tensile testing machine at room temperature. Test specimens are
prepared as per ASTM D 638 standard of type-I. A strain rate of 5mm min1 over a gauge length of 50mm and a
50kN load cell is used for all specimens during the experiment.

Impact test
The Izod impact tests are conducted using Instron make impact testing machine at room temperature. Test
specimens are prepared as per ASTM D 256 standard. Notches are prepared on all specimens as per the standard
by using Instron make notch cutter. During the test, a 10 J capacity hammer was selected for fracture of the
nanocomposite samples.

Micro-hardness test
A Vickers micro-hardness tester, SHIMADZU, of Japan make is employed to study the hardness of PTFE/HNT
nanocomposites. The test parameters considered are 100g load and 15s duration. The indentations are observed
using optical microscope provided with the tester at 400magnification.

Scanning electron microscope (SEM) images


The microstructure images of fracture surfaces of impact and tensile fracture test specimens are captured using
TESCAN SEM. To avoid electrostatic charging during imaging, the fractured surface samples are coated with a
thin layer of gold. The images are captured using 5kV operating voltage at 25000magnification.

Results and discussion

Morphological study
X-ray diffraction analysis (XRD)
For pure HNT, the peak occurs at a basal spacing of 0.719nm (7.19 ) [33]. The peaks of all nanocomposites
consistently showed at the nearly same 2 and are given in table1. The basal spacing of the nanocomposites is
calculated using Braggs law. Intensity counts, inter-planar spacing i.e. d-spacing values for crystalline peaks and
amorphous nature of the nanocomposites are also analyzed. The addition of filler in the matrix material has
shown an increase in the intensity value of the peaks (figure 3(a)) and a maximum intensity value is observed
corresponding to 8 wt% of HNT i.e. for E specimen. From the figure3(b), it is observed that, the addition of HNT
filler in the PTFE matrix, a peak is appeared at about 12.3, in contrast to pure PTFE. A gradual increase in the area
of the peak is observed at different wt% of HNT loading. A maximum increase in the intensity count is observed
for 10% HNT addition which corresponds to a basal spacing of 7.18 .

Differential scanning calorimetry (DSC)


Heating and cooling thermograms are depicted in figures4(a) and (b). PTFE nanocomposites showed no indication
of any additional reaction between the filler and the matrix in the given temperature range and some apparent

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Mater. Res. Express 4 (2017) 045301 S Gamini etal

Figure 3. XRD spectra of PTFE/HNT nanocomposites: (a) crystalline peaks; (b) increase in peak intensity due to wt% HNT
addition at 12.3 two theta.

variation in the position of transition melting peak. From figure4(a), a shift of melting peak is observed [23]. In
the current work, the degree of crystallinity of samples (AF) is calculated using equation(1); H100f for 100%
crystalline PTFE is in the range (57104 J g1)[34]. The H100f of 83 J g1 is selected for this study. From the table2,
neat PTFE depicted degree of ystallinity of 57.83% and PTFE with 10 wt% HNT loading manifested in maximum
degree of crystallinity of 74.7%. The increase in degree of crystallinity, which is a function of heat absorption capacity,
leads to enhanced functional properties. Enhanced degree of crystallinity can be attributed to concentration of HNT
and promotes nucleation process simultaneously at several locations during cooling of the nanocomposites.
The addition of HNTs in PTFE matrix has significantly affected the crystallization behaviour of the PTFE
nanocomposites. From the heating thermograms (figure 4(a)) of PTFE nanocomposites, it is observed that the
melting point temperatures of specimens (B, C, E, F) are slightly affected compared to the neat PTFE. In these
specimens, a new crystal structure may be promoted at the surface of HNT. However, in case of specimen D, the
melting temperature is unaffected by the incorporation of HNT. From cooling thermograms of PTFE nanocom-
posites (figure 4(b)), in case of specimen B, C, and E, the hindering type of crystallization and for specimens D
and F heterogeneous crystallization is observed. In case of heterogeneous crystallization, the nucleation will be
initiated by the HNT filler, whereas in hindering type of crystallization the nucleation will be initiated by the PTFE
matrix region. The discussion presented here is for understanding the nucleation and crystal growth in PTFE nan-
cocomposites only i.e. the changes in the properties of naocomposites are independent of type of crystallization.
In addition, the reduced size of PTFE crystallite is observed for nanocomposite as compared to neat PTFE [35].

Mechanical properties
Dynamic mechanical analysis (DMA)
The variation of storage modulus as a function of temperature (figure 5(a)) shows that the storage modulus of
the material increases as a function of wt % of HNT loading. This shows the enhanced stiffness of the material
on the addition of HNT. The tan plot (figure 5(c)) suggests the possibility of a relaxation present around the
room temperature which corresponds to the relaxation of the polymer. This is due to the change from the
13-CF2-unit helical conformation to 15-CF2-unit helical conformation [36]. The storage modulus has shown
a steady decrease with the temperature whereas the tan delta plot shows a peak maxima at around 120 C
corresponding to alpha glass transition. The tan delta value corresponds to the loss factor of the polymer and
is related to the energy dissipated. The shape and intensity of the tan delta peak gives an indication on the %
crystallinity of PTFE. From figure5(b), it is realized that the loss modulus scales with concentration of HNT
and it reflects the increase in viscous nature of the PTFE nanocomposites. Figure5(c) shows tan as a function
of temperature. From tan studies, no significant variation is found in the glass transition temperature, whereas
slight decrease in the damping property is observed. The variation in the tan is an indicative to the molecular
movement under thermal and mechanical loads and phase transitions of the polymer nanocomposite [23, 37].

Tensile properties
Figure 6 shows the stressstrain diagrams of the specimens AF. The values of yield tensile strength and Youngs
modulus are calculated for each curve and are presented in table2. The increase in wt% of HNT results in an increase
in yield tensile strength and a decrease in ultimate tensile strength (figures 7 and 6, respectively). The yield tensile
strength and Youngs modulus are improved by 135% and 250%, respectively. A similar trend was also found in
literature [38]. During the test, it is noticed that the specimen A (i.e. neat PTFE) deforms steadily and reaches yield
point. However, due to strain hardening, an increase in the applied stress is observed after yield point. Eventually,
it breaks at about 400% strain. The specimens B and D (i.e. low concentration of HNT) depicted initial resistance

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Mater. Res. Express 4 (2017) 045301 S Gamini etal

Figure 4. DSC thermograms of PTFE/HNT nanocomposites: (a) heating scan; (b) cooling scan.

Table 2. Mechanical and thermal properties of PTFE/HNT nanocomposites: A=0 wt%; B=2 wt%; C=4 wt%; D=6 wt%; E=8 wt%;
F=10 wt%.

Mechanical properties Thermal properties

Designation Yield tensile Youngs Impact Vickers % Melting Crystallization Glass transition Heat of
strength modulus strength Hardness crystallinity temperature temperature temperature fusion
(MPa) (MPa) (kJ m2) (MPa) % Xc Tm (C) Tc (C) Tg (C) (J g1)

A 08.820.40 245.5414.19 10.970.42 23.07 57.83 333 310 132.25 31


B 10.450.39 415.5906.67 11.880.97 25.72 63.85 336 308 131.19 33.1
C 10.430.32 521.0626.92 13.470.65 29.20 73.5 337 307 132.18 34.6
D 10.650.26 477.1119.62 11.380.65 25.63 65.06 332 311 131.19 35.1
E 10.350.51 566.3623.62 11.890.72 35.90 72.28 337 308 130.94 36.3
F 11.520.54 607.8030.94 12.980.61 37.61 74.7 334 312 130.95 42.1

till yield point and further elongated uniformly (figure 8). A flat plateau corresponding to this effect is well evident.
Moreover, no substantial strain hardening is observed from the figure6. For sample C, a drop in stress after yield
point is observed, which may be due to the poor adhesion of HNT and PTFE [39]. For samples E and F, an appreciable
decrease in the applied stress is observed after the yield point. This is mainly due to poor dispersion of HNTs in the
PTFE matrix. The ultimate tensile strength and percentage elongation are significantly reduced in comparison to
neat PTFE [40, 41]. The ultimate tensile strength is decreased from 16.48MPa for neat PTFE to 9.72MPa at 10 wt%
of HNT, and percentage elongation is decreased from 392% for neat PTFE to 48% at 10 wt% of HNT.
In case of Youngs modulus, it is clear from the figure9 that the Youngs modulus scales with HNT concentra-
tion. The addition of hard filler in soft matrix can increase the Youngs modulus as well as bulk hardness of the

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Mater. Res. Express 4 (2017) 045301 S Gamini etal

Figure 5. DMA plots of PTFE/HNT nanocomposites: (a) storage modulus and temperature; (b) loss modulus and temperature;
(c) tan and temperature.

nanocompoiste. Moreover, increasing filler content makes the PTFE nanocomposites quasi-brittle [39]. This
behaviour is observed in the specimens E and F. Moreover, increasing filler content develops more interfaces in
the PTFE nanocomposites. Due to poor dispersion and agglomeration of HNTs in the PTFE matrix, the interface
or bonding strength may be poor [40]. Moreover, the cracks may be initiated from these locations, which contrib-
ute less elongation near break point. Figure9 depicts mechanical properties as a function of HNT concentration.

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Mater. Res. Express 4 (2017) 045301 S Gamini etal

Figure 6. Engineering stress-engineering strain diagrams of PTFE/HNT nanocomposites.

Figure 7. Effect of wt% HNTs addition on yield tensile strength.

Figure 8. Neck formation through gauge length on the dog bone test specimen.

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Mater. Res. Express 4 (2017) 045301 S Gamini etal

Figure 9. Effect of wt% HNTs on yield tensile strength and Youngs modulus.

Figure 10. Effect of wt% HNTs on impact strength.

Impact properties
The effect of concentration of HNTs on impact properties of PTFE nanocomposite are shown in table2. Figure10
shows the increase in impact strength corresponding to 4 wt% of HNT. The increase in the energy absorption of
the nanocomposites can be attributed to the dispersion of HNTs in the PTFE matrix and % crystalllinity of the
nanocomposites. The variation in the impact strength is seen from the figure10. The observed impact properties
are in well correlation with % crystallinity [23].

Micro-hardness
Vickers micro-hardness values of the PTFE nanocomposites are presented in table2. The values given in table2
represent the average value of three readings for each nanocomposite sample. The increase in the hardness is
observed due to increase in the wt% of HNTs addition in the PTFE matrix. The increase in these values is due to the
dispersion of hard HNT filler in the soft PTFE matrix. From the table2, the significantly enhanced micro-hardness
of 37.6MPa was realized for specimen F over neat PTFE (23.07MPa) [42].

SEM image analysis


Microstructure of fractured specimens
Figures 11(a) and (b) shows the SEM images of tensile fracture specimen E at two different magnifications.
The gaps between spherulites in the image are an indicative of crack initiation and propagation. Figure12 shows
the SEM images of impact fracture specimens B, C and D. The fracture surfaces revealed the pulling effect

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Mater. Res. Express 4 (2017) 045301 S Gamini etal

Figure 11. SEM images of tensile fracture specimen at 10 wt% HNT: (a) at 1000magnification; (b) 20000magnification

Figure 12. SEM images of impact test fracture surfaces of PTFE/HNT nanocomposites: (a) 2 wt% of HNT; (b) 4 wt% of HNT;
(c) 6 wt% of HNT.

of HNT portion from the matrix material. Figures12(b) and (c) show the uniform pull out regions suggesting
better dispersion of HNT in the matrix. Also from the table2, the impact strength is also high for these samples.
The pulled out effect is displaying in the form of arbitrary shaped gaps in the images. The density and size of
these gaps are different and reveals the dispersion of HNT added to the matrix material [43]. The impact test
specimens are deformed within a short time and therefore exposed to high strain rates during the test. This
increase is due to fibre-related energy dissipation mechanisms, such as fibre debonding, pull out, bridging and
fracture, which induce plastic deformation of the PTFE polymeric matrix before failure. Bridging and fiber
fracture are likely to occur as a consequence of HNT particles with length longer than the critical value for
effective reinforcement, while debonding and fiber pull out are expected to occur as the result of a set of HNTs
with length shorter than the critical value. The increase in the energy absorption of the nanocomposites can be
attributed as a function of dispersion of HNTs filler in the PTFE matrix material and degree of crystalllinity of
the nanocomposites [44].

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Mater. Res. Express 4 (2017) 045301 S Gamini etal

4.Conclusions

The neat PTFE is strengthened with natural mineral halloysite nanotubes. The PTFE nanocomposite sheets of
2%10% with an increment of 2 wt% HNT loading are fabricated. Subsequently thermal and mechanical tests
are conducted and the results analyzed.

The peaks in XRD plots indicated the presence of HNT in the nanocomposites. With the wt% of HNT
increase in the nanocomposites, an increase in the peak size is observed around a 2 theta of 12.3. A
maximum increase in the intensity count is observed for 8 wt% HNT addition which corresponds to a basal
spacing of 7.18 .
DSC results has shown that HNT act as hetero nucleating agent. The HNT content in nanocomposites has
helped in increasing the degree of crystallinity. The degree of crystallinity of PTFE increased from 57.83% to
74.7%.
DMA results shown increase in storage modulus, loss modulus and tan delta values. The variation in the
results indicates that the addition of HNTs has improved the capability of the material to dissipate energy as it
indicates an enhanced loss modulus.
Improved mechanical properties of PTFE/HNT nanocomposites showed an increase in yield tensile strength
by 135% and tensile modulus by 250% in comparison with neat PTFE. Also, an increase in the impact
strength by 130% at 4 wt% loading is observed. The maximum Vickers micro-hardness value is observed
for sample F, which is increased by 163% compared to neat PTFE. From the mechanical analysis, at higher
HNT loading (i.e.>8 wt%), poor dispersion HNT is realized. Moreover, change in PTFE structure is also
observed. The enhancement in mechanical properties can be attributed to increase in degree of crystallinity.
SEM micrographs are shown for impact as well as tensile fracture surfaces. From SEM micrographs, pull out
regions are observed suggesting resistance offered by the HNT in the matrix attributed to good interfacial
strength. This is mainly evident at smaller fraction of HNT (4 wt% to 6 wt%) where, the dispersion of HNT
in PTFE matrix is proper.

Hence, HNTs can be suggested as a reinforcement material for improving several mechanical and thermal
properties of PTFE matrix.

Acknowledgment

The authors would like to acknowledge the funding support from UGC-NRCM. In addition, the authors would like
to thank Ms. Priti Xavier, Department of Materials Engg, IISc, Bangalore for assisting in thermal characterizations.

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