Journal of Inorganic and Organometallic Polymers and Materials

https://doi.org/10.1007/s10904-022-02518-3

RESEARCH

Polymer Blend Nanoarchitectonics with Exfoliated Molybdenum

Disulphide/Polyvinyl Chloride/Nitrocellulose
Pratibha S. Jadhav1 · Shankar S. Humbe1 · Girish M. Joshi1   · R. R. Deshmukh2 · S. Kaleemulla3

Received: 3 July 2022 / Accepted: 8 December 2022

© The Author(s), under exclusive licence to Springer Science+Business Media, LLC, part of Springer Nature 2023

Abstract
Inorganic fillers modified polymer blends are in demands for domestic as well as engineering applications. In the present
investigation, polyvinylchloride (PVC)/Nitrocellulose (NC)/Molybdenum disulphide ­(MoS2) polymer blend were prepared
by solution blending. Chemical functionalities present in polymer blends were confirmed the interaction of filler and polymer
host system analysed by Fourier transform infrared spectrophotometer. E ­ 2g and A
­ 1g active mode of Raman scattering were
analysed by Raman spectroscopy. Increased degree of crystallinity and crystallite size of polymer blends due to incorpora-
tion of ­MoS2 was investigated by X-ray diffraction. Increased pore morphology of polymer blends was foreseen by Scan-
ning electron microscopy. Intercalated layers of ­MoS2 in polymer host system was confirmed by energy dispersive X-ray
analysis. Dielectric properties of the modified blends were studied by impedance analyser. The hydrophobic to hydrophilic
nature of polymer system was determined by measurement of contact angle and relative surface energy analysed by surface
goniometer. Increased thermal conductivity due to interaction of filler and polymer host system mutually correlate to the
increased degree of crystallinity were explored by Lee’s disc probe. We quantified the influence of M
­ oS2 modified polymer
blends could be preferred excellent candidate for engineering domain.

Keywords  Polymer nanocomposites · Nanofiller · PVC · Thermal conductivity · Exfoliated ­MoS2

1 Introduction and nano fillers can have a substantial impact on the char-
acteristics of composite materials. As a result, nano fillers
In the present era of polymer nanocomposites integrated can maintain the workability of polymers that can be easily
with varying grades of nano fillers enabled to deploy for extruded or moulded while also being significantly lighter
emerging applications. Choice of nano fillers employed than traditional polymer composites, which has a substantial
in polymer blends for improved interfacial compatibility environmental impact [3]. The utilisation of nanofillers in
of polymers systems that are incompatible [1]. Nano fill- particular has resulted in the development of improved poly-
ers, often in conjunction with conventional fillers, can dra- meric matrix nanocomposites for the production of high-
matically increase or change optical, electrical, mechani- performance products [4].
cal, thermal, or fire-retardant capabilities of polymers when Fiber-reinforced composites have emerged as the material
incorporated in polymer matrix [2]. Mixing ratio of polymer of choice in the aviation and aerospace industries because of
its great strength performance per unit weight [5]. Polyvinyl
chloride (PVC) and Nitrocellulose (NC) thermoplastic poly-
* Girish M. Joshi mers are compatible. Owing to their inherent properties they
[email protected]
can be utilised for various applications. The properties and
1
Department of Engg. Physics and Engg. Materials, Institute importance of both the polymers was discussed in previous
of Chemical Technology Mumbai Marathwada Campus, report [6]. Based on the information adopted from previous
Jalna, Maharashtra 431203, India report we selected both the polymers for blending purpose
2
Department of Physics, Institute of Chemical Technology, and further in this study we studied their modification by
Matunga, Mumbai 400019, India inorganic filler and effect on their physical and chemical
3
Thin Film Laboratory, Centre for Functional Materials, properties.
Vellore Institute of Technology, Vellore, Tamil Nadu 632014,
India

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 Journal of Inorganic and Organometallic Polymers and Materials

Polymer/inorganic NCs have become a prominent branch excellent EMI shielding property [20]. The preparation and
of physics, materials science, biology, and chemistry among structural property analysis of polymer/MoS2 composites
other subjects, due to their enormous interfacial areas and have been the subject of numerous papers during the past
strong interfacial interactions, which often lead to improved few years. The dispersion of ­MoS2 and the interfacial inter-
properties and even novel functions when compared to cor- actions between the polymer matrix and ­MoS2 are thought to
responding components [7, 8]. Nanocomposites are made up be the most important factors to improve the characteristics
of two or more phases with various compositions or struc- of polymer materials, similar to other 2D nanofillers. Table 1
tures, at least one of which is between 10 and 100 nm in size. summarise the literature study of ­MoS2 modified polymer
Due to the small number of atoms per particle and potential composites. Keqing zhou and team constructed polystyrene/
for differing properties from the bulk material, fillers with MoS2 by using latex technology and self-assembly of oppo-
particle sizes in the nanometre range may exhibit intense sitely charged M­ oS2 on polystyrene surface. They observed
interactions with the matrix [9]. Many composite materials, the improved fire safety and thermal stability of polystyrene
made of two or more constituents, have been designed that due to the addition of M ­ oS2 [21]. Similarly, M­ oS2 showed
have chemical and physical properties that are significantly impact on thermal and mechanical properties of PVA uti-
different from those of the individual ingredients [10]. When lised for engineering membrane applications [22]. Recently,
developing polymer composites, the proper selection of 2D Jin Yang and his research team showed that CF-MoS2 hybrid
nanosheets makes it easier to improve the composites' many material can be utilised to improve tribological and mechani-
properties, such as their dielectric, heat conductive, elec- cal properties of materials [23]. Similarly, ­MoS2 modified
tromagnetic interference shielding, or mechanical proper- PTFE polymer composite showed improved lubrication
ties [11]. The exponential expansion of optoelectronic and properties of PTFE which will be feasible for bearing appli-
nano electronics has sparked a new area of research replac- cations [24]. PDA/PMA/MoS2 polymer composites can be
ing graphene with new two-dimensional (2D) materials. used as adsorbent for removal of cooper ions [25]. He-Xin
Among, the transition metal dichalcogenides molybdenum Zhang et al. reported in-situ polymerization technique to
disulphide (abbreviated as ­MoS2) attracted much attention develop ­EMoS2 based nanocomposite with polyethylene
due to their emerging properties [12]. ­MoS2 is a 2D material (PE). The resultant PE/MoS2 nanocomposite exhibited
with layered structure comparable to graphene. It is made up enhanced thermal and mechanical properties [26]. Junjie
of covalently bound Mo and S atoms. Formation of M ­ oS2 Guo et al. suggested conventional scotch tape approach to
molecular layer, two hexagonal S atomic layers sandwich a produce PVA/MoS2 polymer nanocomposite. The modified
plane of Mo atoms, forming three planes of atoms. These composite exhibited improved electrical properties which
layers are linked by weak Vander Waals connections, mak- will be feasible for field effect transistors [27]. Rajeev Ray
ing it simple to slide and separate [13]. It possesses a large et  al. reported the improved performance and moisture
specific surface area, superior mechanical properties, and a stability of perovskite solar cell of poly(3-hexylthiophene-
substantial elastic strain, allowing it to maintain a low fric- 2,5-diyl) by using 2D-MoS2 nanohybrid [28]. Abdul Saboor
tion coefficient and excellent lubricating capabilities even in et al. produced PS/PANI/MoS2 polymer nanocomposite by
vacuum and at high temperatures [14]. As an innovative 2D using solution casting method. The resultant composite pos-
layered nanomaterial exfoliated ­MoS2 nano sheets, have out- sesses high electrical conductivity and dielectric behaviour
standing thermal properties, making them a suitable choice for EMI shielding effectiveness [29]. Keqing Zhou et al.
for thermal property application in polymers [15]. Some reported in-situ emulsion polymerization of polymethyl-
studies have shown including exfoliated ­MoS2 nano sheets methacrylate (PMMA)/MoS2 nanocomposites. Modified
at extremely low loading can endow polymer matrices with nanocomposite exhibited improved thermal stability with
notable thermal and mechanical properties in recent years 1% addition of ­MoS2 [30].
[16]. The bulk M ­ oS2 sheets are commonly sonicated in sta- In the present study, we studied how M ­ oS2 can change
bilising liquids, such as solvents or aqueous surfactant solu- character of a PVC/NC polymer blend for various applica-
tions, during the exfoliation process. Then, between sheets, tions. Polymer blend was prepared by using solution blend-
weak van der Waals forces are disturbed. As a result of the ing and casting method and further modified by ­MoS2. The
contact with the liquid, two-dimensional M ­ oS2 nano sheets structural and morphological issues were reported in detail.
are formed and stabilised against aggregation. Recently Both thermal and engineering responses increase at the opti-
Karolina Wenelska et al., prepared polyethylene nanocom- mum concentration of ­MoS2, which could be related to the
posites with exfoliated M ­ oS2 as nano filler, demonstrated creation of a good network of nano filler inside the polymer
enhanced thermal stability, thermal conductivity and fire matrix. The average thickness of PVC/NC/MoS2 hybrid pol-
retardancy [17–19]. Abdul saboor and his team developed ymer composite thin films (free standing) is 0.1 mm, which
PS/PANI/MoS2 polymer composite which possesses high is extremely thin. The current study explored as new hybrid
dielectric constant and high electrical conductivity exhibits polymer blend for engineering applications.

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Journal of Inorganic and Organometallic Polymers and Materials

Table 1  Literature survey of ­MoS2 modified polymer nanocomposites and blends

Name of polymer composites Synthesis techniques Properties Applications References
and blends

Polystyrene/MoS2 Latex technology and Thermal stability and fire Fire retardant and thermally [21]
self-assembly method safety stable
PVA/MoS2 Solution cast Thermal and mechanical prop- Engineering membrane [22]
erties good dispensability
PI/CF/MoS2 in-situ emulsion polymeriza- Tribological properties To improve the anti-friction of [23]
tion Mechanical &chemical proper- composite stern bearings
ties
PTFE/MoS2 Taguchi method Lubrication property and wear Bearing application [24]
and injection moulding resistance
Tribological properties
PDA/ PMA/ ­MoS2 Surface initiated Thermodynamics, adsorption Used as adsorbent for Removal [25]
atom transfer radical kinetics, isotherms of copper ions
polymerization
PE/MoS2 In-Situ polymerization Thermal – [26]
stability and mechanical
properties
PVA/MoS2 Conventional scotch-tape Electrical properties Field effect transistor for inte- [27]
approach grated circuits and sensors
poly(3-hexylthiophene- Solution blending Electrical properties Improving performance and [28]
2,5-diyl)/MoS2 moisture stability of perovs-
kite solar cells
PS/PANI/MoS2 Solution cast Dielectric properties and AC EMI shielding effectiveness [29]
conductivity
PMMA/MoS2 Emulsion polymerization Thermal stability – [30]

2 Experimental Details PVC and NC solutions were mixed together by stirring

(at 600 rpm for 2 h) to obtain PVC/NC polymer solution.
2.1 Materials ­MoS2was mixed in 10 ml THF and sonicated (30 min at
room temperature 3­ 00C). Then the dispersed M
­ oS2 in THF
Polyvinyl chloride (PVC) polymer granules were procured was added to PVC/NC solution and stirred (at 400 rpm
from Technovinyl polymers Ltd., Mumbai, India, with for 1 h) to obtain ­M oS 2 homogeneity of PVC/NC solu-
molecular weight 233,000 g/mol and with tensile strength tion. Then the obtained solution was poured in glass petri
22.8 MPa, volume resistivity 8 × 1014 Ω/cm and specific dish and kept for complete evaporation of THF1(10 h).
gravity of 1.38(± 0.03). Nitrocellulose (NC) of HM 10/25 The whole reaction was carried out at room tempera-
grade was used for the preparation. It was supplied by GRN ture(30 °C). Table 2 summarises sample configurations of
cellulose PVT Ltd., Ramnagar chandauli in cotton form. PVC, NC and ­MoS2 used for blending purpose. Further,
Molybdenum disulphide of Moly Tech super fines grade obtained PVC/NC/MoS2 polymer blend sample was uti-
was procured from Asbury graphite mills, INC (a division lized for the different characterizations.
of Asbury carbons). Tetrahydrofuran (THF) of AR grade
was procured from S. D. fine chemicals, Ltd., Mumbai, India
which is used as solvent.
3 Characterization Techniques
2.2 Preparation of PVC/NC/MoS2 Blends
3.1 Fourier Transform Infrared Spectroscopy
The modified PVC/NC/MoS2 blends with 2.5,5,7.5,10%
loading of M
­ oS2 was prepared by solution casting. Fig- A Jasco Fourier Transform Infrared Spectrophotometer
ure  1 demonstrate the basic protocol and interaction 6600 (JASCO FT/IR-6600) was used to determine FT-IR
model of PVC/NC/MoS2 composite films. Initially, Sepa- spectra of PVC/NC/MoS2 polymer blends in the range of
rately, PVC and NC were mixed in THF. and stirred (at 4000–400 ­cm−1. As result of this, a suitable PVC/NC and
600 rpm for 3 h) till the complete dissolution. Then the PVC/NC/MoS2 mix was verified.

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 Journal of Inorganic and Organometallic Polymers and Materials

Fig. 1  Protocol and proposed

model of PVC/NC/MoS2 poly-
mer blends

Table 2  Composition of PVC, NC and ­MoS2 in different weight frac- 3.5 Electrical Study

tions
Sample code Polymer blend Filler (wt.%) Dielectric studies of materials were done by using a dry
temperature calibrator and a PSM-1735 (Newtons4th, UK)
PVC NC MoS2
impedance analyser (frequency range of 10 Hz to 10 kHz
(NC5) 95 2.5 2.5 and temperature range of 30 to 150 OC) (ALAB Instru-
(NC6) 90 5 5 ment). For test, a sample with a thickness of 100 mm and
(NC7) 85 7.5 7.5 diameter of 10 mm of polymer film was kept in the fixture.
(NC8) 80 10 10

3.6 Surface Contact Angle

3.2 Raman Spectroscopy
The contact angle and surface energy of polymer films
The Raman spectra was recorded on Renishaw InVia Raman were evaluated using sessile drop method. A contact angle
Microscope. The 785 nm exiting wavelength laser was used. goniometer (DMe-211 Plus (Kyowa Interface Science
Laser power was used as 1 mw. The spectra were recorded Co., Ltd.)) was used to measure contact angle of PVC/
in 0–3000 ­cm−1 of Raman shift. NC/MoS2 blend at room temperature. For measurement
of surface energy two liquids with different polarity water
(γ = 72.8 mN ­m−1) and diiodomethane (γ = 50.8 mN m ­ −1)
3.3 X‑Ray Diffraction Analysis were used. For measuring static contact angle 2.5  ml
micro drop of liquid was poured on surface of polymer
XRD characterization of samples was performed by using film. liquid droplet was captured by computer-controlled
Bruker AXS D8focus advance XRD meter (Rigaku, Japan, camera, and Contact angle data were automatically col-
Tokyo), Cu Kα radiation with wavelength of λ = 1.54 Å pro- lected. Measurements were repeated for five times at dif-
duced with current of 40 mA and potential difference 40 kV. ferent place. Then the mean value was computed. Fur-
The diffraction angle was used in range of 10° to 80°. thermore, surface energy was then calculated using the
Owens–Wendt–Rabel–Kaelble and Wu method.

3.4 Scanning Electron Microscope

3.7 Thermal Properties
Scanning electron microscope images of mixes were exam-
ined using EDAX analysis on a Zeiss SEM (EV108). Sur- Lee’s disc method was used to optimise thermal conductiv-
face images were taken in a 10 m scale range at a 5–10 kV ity of PVC/NC/MoS2 polymer blend samples at room tem-
accelerating potential. perature. Each sample was tested at least three times and the

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Journal of Inorganic and Organometallic Polymers and Materials

average value was used as final reading. All the measure- resulted in various improved properties was discussed above
ments were started at room temperature (30 °C). in literature study table.

4.2 FTIR Analysis of PVC/NC/MoS2 Polymer Blends

4 Results and Discussion The intermolecular interactions between various compo-

nents are substantially influences on the characteristics of
4.1 Role of ­MoS2 as Dopant composite materials. The use of vibrational spectroscopy is
a common method of studying intermolecular interactions.
Molybdenum disulphide ­(MoS2) belongs to transition metal However, FTIR spectroscopy allows for a quick and simple
dichalcogenide family with a chemical structure similar to evaluation of the interaction. FTIR was conducted to confirm
­WS2. Molybdenum disulphide ­(MoS2) crystals are hexagonal chemical fingerprints of PVC/NC blend modified by ­MoS2.
layered structures in which atoms in layer are connected with For PVC/NC virgin blend, chemical composition was dis-
strong covalent bonds with weak Van der Waals forces like cussed in our previous report [6].
graphite and h-BN [31]. The layers are compacted together Figure 2a–d illustrate FTIR spectra of all PVC/NC/MoS2
to form a sandwich structure with weak bonding. The novel (2.5,5,7.5,10%) polymer blend. In the IR spectrum of PVC/
sandwich construction could be useful in a variety of situ- NC/MoS2(2.5%) blends sharp peak present in the range
ations. Super lubricant, sensors, batteries, photo catalyst of 600–700  ­cm−1 assigned to C–Cl symmetric stretching
and other technological sectors where M ­ oS2-based polymer bond, 965 ­cm−1 corresponds to C–H wagging due to PVC.
composites are used for hydrogen storage and blends [32]. The peak at 1386 ­cm−1 could be attributed to C=H stretch-
Because of its unique properties, ­MoS2 has gained a lot of ing vibrations. The peak present at 1718 ­cm−1 assigned to
attention in recent years. Qualities arising from its struc- carbonyl(C=O) stretching vibrations which indicates suc-
ture results in remarkable optical, thermal, and mechanical cessful formation of PVC/NC/MoS2 polymer composites.
properties. The reason for choosing ­MoS2 is it blends very The peak present at 2859 ­cm−1 and 2936 ­cm−1 is assigned
easily in solution and it has excellent film forming proper- to ­sp3 C–H in phase and out of phase stretching vibrations
ties. ­MoS2-based polymer composites are a new class of respectively shown in Fig. 2a. Furthermore, with the higher
materials that combine appealing functional features of addition(10wt%) of ­MoS2 major changes was observed
­MoS2 (electrical, optical, thermal, mechanical, etc.) with the in the intermolecular hydrogen bonding of pure PVC as
benefits of polymers [33]. Low cost and processability these depicted in Fig. 2b. The intensity of C–Cl bond reduced in
are two advantages of ­MoS2 modified polymers blends and PVC/NC/MoS2 blends indicates that part of chlorine was
composites. Various reports have studied the effect of ­MoS2 removed as the ­MoS2 loading increases. Also, the C–H peak
on different properties of polymer composites. Some of the intensity was reduced as ­MoS2 loading increased. Moreo-
recent reports on M ­ oS2 based polymer nanocomposites ver, the peak present at 1276 ­cm−1 and 1387 ­cm−1shifted

Fig. 2  FTIR spectra of PVC/NC/MoS2 polymer blends in a 500–3200 ­cm−1, b 500–1500 ­cm−1 range

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 Journal of Inorganic and Organometallic Polymers and Materials

to 1218  ­cm−1 and 1375 ­cm−1 respectively at higher load- is method based on active mode of Raman scattering that
ing of M
­ oS2 resulted in successful modification of PVC/NC uses laser light to interact with molecular vibrations/phon-
polymer blends. It can be observed that after incorporation ons and shifts the energy of laser photons up and down [35].
of ­MoS2 there is an interaction between ­S2− of ­MoS2 with The energy shift in traditional Raman spectroscopy is used
­H+ of PVC making the hydrogen bonding between PVC/NC to determine the vibrational modes in system. It is the most
and ­MoS2 [34]. The reduced peak intensity corresponds to attractive method for characterising carbon compounds,
incorporation of ­MoS2 and the reduction of PVC content in because of its non-destructive, rapid, and high-resolution
blend system. Table3 displays the wavenumbers and their assessment, it provides electronic and structural information.
corresponding bond assignments. The interactions on molecular structure of an element
in composites were demonstrated using this technique [3].
4.3 Raman Spectroscopy of PVC/NC/MoS2 Polymer Figure  3a–d displays Raman spectra of pure PVC, NC,
Blends ­MoS2 and PVC/NC/MoS2 polymer blends. The spectra
were recorded with 785 nm wavelength laser, 1 mW power
Raman spectroscopy is the most attractive approach for char- with 10 acquisitions. Raman spectra shown in Fig. 3a. shows
acterising carbon compounds. Because of it’s non-destruc- main characteristic bands for PVC which is mutually cor-
tive, rapid, and high-resolution investigation, it provides responding with other reports. Spectrum shows high inten-
electronic and structural information. Raman spectroscopy sity Raman bands in range of 600–700 ­cm−1 corresponds
to C–Cl bond stretching vibration. The band at 1325 ­cm−1
and 1430 indicates alkyl (CHn) and D band respectively. The
Table 3  FTIR for PVC/NC/MoS2 polymer blends band present at 2913 ­cm−1 assigned to C-H stretching vibra-
Wavenumber ­(cm−1) Bond assignments tion in ­CH2 structural fragment [36, 37]. Figure 3b. presents
Raman spectra for NC. The highly intense peak at 840 ­cm−1,
610, 710 C–Cl symmetric stretching 1284 ­cm−1 and 1660 ­cm−1 corresponds to ­NO2 symmetric
965 C–H wagging stretch of nitrocellulose [38, 39].
1386 C=H stretching Raman spectra of pure ­MoS2 can be shown in Fig. 3c.
1718 (C=O) Carbonyl stretching Basic two characteristic peaks at 382 ­cm−1 and 407 ­cm−1
2859, 2936 C–H in phase and out of corresponds to in-plane and out of plane of E ­ 2g and A
­ 1g
phase stretching
vibrations of M ­ oS2 respectively. The E ­ 2g mode involves

Fig. 3  Raman spectrum of
a virgin PVC b pure NC, c
virgin ­MoS2, d PVC/NC/
MoS2(2.5,5,7.5,10 wt%) poly-
mer blends

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Journal of Inorganic and Organometallic Polymers and Materials

inlayer Mo and S atom displacements due to phonon mode, ­MoS2. The existence of characteristics peaks and diffrac-
whereas the ­A1g mode includes out-of-layer symmetric S tion angles for virgin PVC and virgin PVC/NC blend was
atom displacements due to vibration along the c axis [40]. discussed in previous report. The decreased crystallinity
The number of layers in ­MoS2 was indicated by the differ- and interplanar spacing was observed for higher amount of
ence of intensities between ­E2g and A1g mode. Figure 3d NC [6]. The sharp characteristic diffraction peaks of pure
represent the Raman spectra for PVC/NC/MoS2. The spec- ­MoS2 around 2θ = 14°, 32°, 39°, 42° depicted in Fig. 4a.
trum of PVC/NC/MoS2 exhibits the sum of both polymers It implies M­ oS2 is highly crystalline in nature and indi-
and nanofiller with significant shift in peak position or cates stacked layered structure. However, the reflections
without any new peaks. It can be seen that Raman peaks at of the lattice planes in the bulk M ­ oS2 material revealed
380 ­cm−1 and 405 ­cm−1 is corresponding to ­MoS2 ­E2g and multiple peaks, indicating the existence of many layers
­A1g modes ­respectively. It confirms successful incorporation of ­MoS2. Figure 4b displays diffractograms obtained for
of ­MoS2 within PVC/NC blend. The ­E12 g and A1g peaks of different amount of ­MoS2(2.5,5,7.5,10 wt%) in PVC/NC/
­MoS2 in blend sample shifted by 5–10 ­cm−1 to a higher fre- MoS 2 polymer blends respectively. However, the new
quency with increased amount of ­MoS2, indicating the pres- characteristic peak appeared at 2θ = 15°was attributed
ence of few layers or exfoliated ­MoS2 layers. The peak pre- due to ­M oS 2 which clearly indicates presence of ­M oS 2
sent at 600–700 ­cm−1 in PVC/NC/MoS2 corresponds C–Cl in PVC/NC blend. Further peak intensity was increased
stretching of PVC. Further the C–Cl peak intensity reduced for higher loading of ­M oS 2. The XRD spectra of PVC/
which indicates the partial removing of Cl atoms from PVC/ NC/MoS 2 shows appearance of some new peaks due to
NC/MoS2 blends which is also confirmed from FTIR and ­MoS2. The main diffraction peak at 2θ = 29° corresponds
EDAX. The weak band present at 2910 ­cm−1 assigned to to PVC started disappearing as ­MoS2 loading increased.
­CH2 stretching vibration of PVC which also started disap- From these results we note that crystallinity was slightly
pearing as amount of M­ oS2 ­increases. It confirms that PVC/ increased for higher amount of ­MoS2 it is consistent with
NC polymer blends was sensitive to addition of ­MoS2. reported ­literature. ­MoS2 can act as nucleating agent with
increasing crystallinity of polymer blends [41]. The crys-
4.4 XRD Analysis of PVC/NC/MoS2 Polymer Blends tallite size was calculated by using the Debye sheerer for-
mula followed from reported literature [42]. In comparison
The crystalline and amorphous phase nanoparticles can to host polymer system crystallite size was increased with
be identified by wide angle X-ray diffraction (WAXD). increased amount of ­MoS2. It was increased from 25.9 to
Bragg's law was used measure the spacing between the 39.9 nm. The degree of intercalation/exfoliation can be
crystalline layers to analyse the crystalline phases of nano- determined by tracking the position of the characteristic
particles. The position, broadness, and intensity of the dis- peak in blends. In the present investigation d-spacing was
tinctive peak in the XRD spectra changes as the distance increased with increased amount of M ­ oS2. Because the
between layers changes; the position of the XRD peak per- structure is chaotic in an exfoliated blends [3]. Table 4
mits determining the type of blends generated. Figure 4a, b displays d-spacing, crystallize size, and degree of crystal-
depicts the XRD patterns of pure PVC, PVC/NC and pure linity of the PVC/NC/MOS2 polymer blends.

Fig. 4  X-ray diffractograms a pure virgin, ­MoS2 and PVC/NC, b PVC/NC/MoS2(2.5,5,7.5,10%) polymer blends

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 Journal of Inorganic and Organometallic Polymers and Materials

Table 4  XRD analysis of PVC/NC/MoS2 polymer blends NC/MoS2 (2.5wt%) polymer blends system. While, in case
Sample details (wt%) Crystallite size Inter- Degree of
of high wt.% dispersion of M ­ oS 2 (10wt%) morphology
D (nm) planar crystallinity was quite different shown in Fig. 5b. The morphological
spacing (%) variation of virgin PVC/NC polymer blend were reported
d ­(A0) in previous work. Increased number of pores was observed
PVC/NC/MoS2 25.9 6.07 34.6 by an inclusion of NC [6]. Pore size was increased from
(95/2.5/2.5) 20 to 36 μm for dispersion of 2.5 wt.% to 10wt% ­MoS2 in
PVC/NC/MoS2 37.7 6.09 31.9 polymer blends s­ ystem. Hexagonal structured pores with
(90/5/5) increased porous size look like honeycomb, were clearly
PVC/NC/MoS2 38.1 6.21 40.1 depicted at higher loading may due to incorporation of
(85/7.5/7.5)
inorganic nanofiller and intrinsic property of material.
PVC/NC/MoS2 39.9 6.23 45.5
Hydrogen bonding between polymer host system and nano
(80/10/10)
entity confirmed by FTIR could be one of the reasons for
increased porous size [43, 44].
Elemental analysis of modified polymer blends was
4.5 Scanning Electron Microscopy of PVC/NC/MoS2 done by using EDAX. It was used to determine the com-
Polymer Blends position of elements present in the blend systems [45].
Figure 6a, b demonstrate the EDAX images of PVC/NC/
Modified surface morphology due to incorporation of nano MoS2 (2.5 and 10 wt%) blend systems. Results confirmed
filler was achieved by scanning electron microscopy shown the presence of C, O, Cl elements with an atomic mass
in Fig. 5a, b. In the present investigation morphology of percent 83, 9 and 6% on addition of 2.5 wt% ­MoS2. While,
2.5 and 10 wt.% of M ­ oS2 dispersed in PVC/NC polymer high amount of M ­ oS2(10 wt%) exhibits the presence of C,
host system has been studied. As depicted in Fig. 5a dis- O and Mo atoms with atomic mass 61,31 and 75% respec-
tribution of porous pattern was observed regularly in PVC/ tively. Presence of Mo atom confirmed composition based
of ­MoS2 dispersed PVC/NC blend system.

Fig. 5  SEM micrograph
images of a PVC/NC/MoS2
(95/2.5/2.5wt%) b PVC/NC/
MoS2 (95/2.5/5wt%) polymer
blends

Fig. 6  EDAX images of images of a PVC/NC/MoS2 (95/2.5/2.5wt%) b PVC/NC/MoS2 (95/2.5/5wt%) polymer blends

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Journal of Inorganic and Organometallic Polymers and Materials

Fig. 7  Dielectric constant of PVC/NC/MoS2 a 95/2.5/2.5 b 90/5/5 c 85/7.5/7.5 d 80/10/10 wt.% polymer blends

4.6 Dielectric Properties of PVC/NC/MoS2 Polymer blend films offers enhanced εr due to interfacial polariza-
Blends tion while at higher frequency dielectric response reduced
[47]. Dipoles gets sufficient time to orient themselves at
Electrical properties were disclosed to know the role filler in lower frequency which results in interfacial polarization
blend system. Figures 7, 8a–d displays dielectric constant(εr) based on Maxwell–Wagner (M-W) model [48]. However,
and loss of PVC/NC/MoS2 polymer blend system. The third at higher frequency polarization trend was decreased due
component of nanofiller may also be added to make poly- to short interval of time for polarization. M-W polariza-
mer blend more conductive or dielectric in nature. M ­ oS2 is tion effect caused by both (conductor–insulator) interfaces
often used as more competitive candidate for devices with were responsible for the enhancement of dielectric con-
enhanced dielectric constant and AC conductivity. stant at lower frequency [49].
It is 2D material with layered structure having nor- The dielectric loss (tan δ) is a material property that
mal fermions with parabolic energy dispersion. which evaluates energy dissipation induced by the migration or
is best comparable to graphene. ­MoS2 is semiconductor rotation of molecules when they are exposed to an electric
with finite band gap ~ 1.2 eV. Hence broadly used to alter field. Figure 8a–d depicts dielectric loss graphs of PVC/
electrical and optical properties of polymer composites NC/MoS2 polymer blend films with frequency (10 Hz to
[20]. εr was calculated using formula taken from literature 10 MHz) at different temperature(30°–200 °C). tan δ for
report [46]. Figure 7a–d represents ε r response of PVC/ 2.5wt% loading of M ­ oS2 was found to be ~ 3.8 shown in
NC/MoS 2 blends with frequency (10 Hz to 10 MHz) at Fig. 8a. It was observed that there is no significant change
different temperature (30–200 °C). ε r of PVC/NC/MoS2 in dielectric loss as a function of ­MoS2 loading. At lower
blend film was found to be ~ 7(10 Hz, 200 °C) at 2.5 wt. % frequencies dielectric loss was observed high this may due
loading of M­ oS2; and for 5 and 7.5 wt.% it remains s­ ame. to interfacial polarization or maxwell–Wagner-Silar’s effect
Further it was increased up to 42% on addition of 10 wt. [50]. As a result, the ­MoS2 layers exfoliated in the PVC/
% ­MoS2. It was observed that at lower frequency region NC blend system enhances the interfacial synergy between

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 Journal of Inorganic and Organometallic Polymers and Materials

Fig. 8  Dielectric loss of PVC/NC/MoS2 a 95/2.5/2.5 b 90/5/5 c 85/7.5/7.5 d 80/10/10 wt.% polymer blends

the nanofiller and the polymers and provides a significant [51]. Pure PVC shows hydrophobic nature further changed
interfacial polarisation at lower frequencies. to hydrophilic after NC blending and even more hydrophilic
nature was observed due to loading of ­MoS2 in PVC/NC
4.7 Surface Properties of Surface PVC/NC/MoS2 polymer blends.
Polymer Blends In case of polymers surface energy(SE) is generally low
as compared to metals. [52]. SE for PVC/NC/MoS2 polymer
The tribological characteristics of liquids are influenced by composites were computed using the Owens Wendt-Rabel-
their wetting behaviour towards sample surfaces. Contact Kaelble (OWRK) and Wu methods. We observed slight dif-
angle (CA) measurements were performed with various liq- ference in SE values using different methods. The contact
uids (pure water, formamide, ethylene glycol, diiodomethane angles of two different liquids, one polar: water, and one dis-
at room temperature). Three measurement was taken at dif- perse: diiodomethane, were employed in this method to cal-
ferent position for each sample. The CA of a water droplet culate total surface energy. Choice of liquids is, ore impor-
and other liquids on the PVC/NC/MoS2 polymer composites tant while obtaining the surface energy. Figure 9b represents
was used to determine the wettability of the sample surface. the SE of PVC/NC/MoS2 polymer blends. Improved SE was
Figure 9a indicates CA of PVC/NC/MoS2 polymer compos- observed as consequence of M ­ oS2 ­loading. However, similar
ite is lower than pure PVC/NC blends for all liquids. trend was observed for all methods with quite similar values.
Recently PVC/NC blends demonstrated hydrophilic prop- SE improved over the surface through bonding interaction
erties. Decreased CA may be due blending of NC. Addition- i.e., hydrogen bonding between filler and polymer blends.
ally, decreased CA of PVC/NC/MoS2 was observed as load- The variation of CA and SE for PVC/NC/MoS2 blends rep-
ing of M ­ oS2 increased. Decreased trend of CA was due to resented in Fig. 9a, b. Although hydrophobic polymers are
increased number of hydrophilic or polar functional groups. used in the great majority of applications Surface interface is
The modifications caused by the insertion of hydrophilic equipped with hydrophilic qualities, which is not achievable
functional groups such as carbonyl, carboxyl, amino, and with hydrophobic polymers. liquid attraction, extraction,
hydroxyl groups resulted in wettability changes in polymer wetting, and spreading require hydrophilic polymers [53].

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Journal of Inorganic and Organometallic Polymers and Materials

Fig. 9  Surface properties of PVC/NC/MoS2 blends a Contact angle b Surface energy

4.8 Thermal Conductivity of PVC/NC/MoS2 Polymer for obtained PVC/NC/MoS2 polymer blends. K was found
Blends to be increased with increased loading of M ­ oS2 in PVC/
NC blend. M ­ oS2 is thermally conducting material, hav-
Knowing thermal transport in polymers is critical for a vari- ing high k i.e., 83–131 W ­m−1 ­k−1 which can increase k of
ety of applications, including new optoelectronic and elec- polymer blends after inclusion and also improves thermal
trical devices. Low thermal conductivities(K) in the order stability of material. Piotr Homa et al. reported increased
of 0.1 W  ­m−1 ­K−1 prevent polymer materials from being k of poly (lactic acid)/CNT/MoS2 due to incorporation of
used in these devices, resulting in poor heat dissipation. As a ­MoS2. The resultant composites value added 65% improve-
result, there have been significant attempts to improve poly- ment in thermal conductivity over pristine sample [57].
mer thermal transfer properties. In the present investigation Moreover, Helio Ribieiro reported impact of h-BN and
we obtained k values by using Lee’s disc method and for- ­MoS2 on improved k of polyurethane (PU). They observed
mula used in previous report [6, 54]. Recently Humbe et al. PU/MoS2 showed higher k i.e., 0.42 W/m. k as compared
reported thermal conductivity of PVDF/PSF/BN polymer to PU/h-BN i.e., 0.23 W/m. k with 0.5wt% of nanofiller
composite by Lee’s disc method [55]. [58].In the present study sample thickness was taken as
Same method was used by Duncan price and his team two folds of 100 μm and diameter is about 2 cm. K was
to measure the k values of polytetrafluorethylene (PTFE) obtained at room temperature(300C). k values enhanced
and PTFE composites [56]. Figure 10a depicts k values from 0.17 ± 0.0085 ­Wm−1 ­k−1 to 0.27 ± 0.0135 W ­ m−1 ­k−1

Fig. 10  a Thermal conductivity of PVC/NC/MoS2 polymer blends b relation curve between specific heat and thermal diffusivity of PVC/NC/
MoS2 polymer blends

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 Journal of Inorganic and Organometallic Polymers and Materials

Table 5  Thermal properties of Name of sample Thermal conductiv- Thermal diffusiv- Specific heat capac- Thermal
the PVC/NC/MoS2 polymer ity (W/m k) ity ­(m2/s) ity (J/Kg k) resistivity (m
blends k/W)

PVC/NC 0.17 286.5 2884.64 5.8

(95/2.5/2.5%)
PVC/NC (90/5/5%) 0.22 370.8 1914.704 4.5
PVC/NC (85/7.5/7.5%) 0.25 421.4 1686.256 4
PVC/NC (80/10/10%) 0.27 455.1 1595.264 3.7

as amount of increased loading of M ­ oS2 with respect to the with increased diameter of pores was revealed by scanning
neat PVC/NC polymer blends. This is mainly due to the electron microscopy. The dielectric study was done by using
incorporation of ­MoS2 in PVC/NC polymer blends sample. impedance analyser. It was observed that dielectric con-
In addition the higher nitrogen content present in NC could stant was slightly increased on the incorporation of ­MoS2.
be responsible for increased K values [59]. On the other Decreased contact angle and enhanced surface energy was
hand, intermolecular interactions such as hydrogen bond- measured by surface goniometer. The hydrophobic nature of
ing and interactions can reduce phonon scattering, result- the polymer blends was turn into hydrophilic with increased
ing in higher thermal conductivity. Moreover, the increased amount of M ­ oS2. Thermal conductivity measured by Lee’s
crystallinity was also responsible for the increased thermal disc method was increased with addition of ­MoS2. Owing
conductivity of polymer composites [60]. Crystallinity to this enhanced thermal performance we can say that M­ oS2
was determined by x-rd. Along with thermal conductivity nanolayers were uniformly distributed in the PVC/NC pol-
specific heat ­(Cp) and thermal diffusivity (α) for PVC/NC/ ymer blends, resulting in a variety of proposed candidate
MoS2 was obtained. α refers to the rate at which heat moves blend for engineering applications.
through a sample, and it is closely related to thermal conduc-
Acknowledgements  The authors would like to gratefully acknowledge
tivity, therefore the two terms can be used interchangeably the Institute of Chemical Technology Mumbai Marathwada Jalna for
[61]. Whereas, ­Cp of a material is defined as the amount of providing a doctoral fellowship. Research scholar Pratibha S. Jadhav
heat (J) absorbed per unit mass (kg) when its temperature is grateful to the Vellore Institute of Technology, Vellore (India), for
rises 1 K (or 1 °C), and it is measured in J/ (kg K) or J/ (kg providing the SEM characterisation facility.
°C). Figure 10b depicts the relation curve between Cp and Author Contributions  PSJ: synthesis and manuscript writing, interpre-
α. From the curve it was observed that ­Cp decreased while α tation of data. GMJ: final analysis, supervised the work. SSH, RRD,
increased with the increased amount of ­MoS2. The obtained and SK: helped in characterization.
value of α for 2.5wt% ­MoS2 was 286.5 ± 14.32 ­m2/s while,
Funding  The authors acknowledge funding from the Institute of Chem-
for 10wt% ­MoS2 it was increased up to 455.1 ± 22.75 ­m2/s. ical Technology Mumbai Marathwada Jalna.
­Cp was increased from 2884.6 ± J/Kg. k to 1595.2 ± 79.76 J/
Kg. k for 2.5wt% and 10wt% respectively. These increased Declarations 
physical properties resulted in good dispersion of M ­ oS2 in
PVC/NC polymer matrix. Due to increased thermal con- Conflict of interest  We all authors have no conflict of interest.
ductivity polymer blends could be utilised for engineering
applications. Table 5 displays the thermal properties of PVC/
NC/MoS2 polymer blends.
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