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Received: 21 December 2021 Revised: 9 February 2022 Accepted article published: 21 February 2022 Published online in Wiley Online Library:
Abstract
In this study, we prepared Polyvinyl chloride (PVC)/Nitrocellulose (NC) polymer blend by the solution casting technique. The
structural properties and decreased interplanar spacing and crystalline nature of the PVC/NC blends were confirmed by an
XRD technique. Basic chemical fingerprint regions of PVC/NC blends were confirmed by the Fourier transform IR method. Opti-
cal properties correlated with a decreased direct and indirect bandgap energy of PVC/NC were estimated using UV–visible spec-
tra. They exhibited a shift in the absorption spectra towards the longer wavelength region due to process of charge transfer in
the blend system. An increased microporous nature of the blends was demonstrated by SEM. Based on the Maxwell–Wagner
model the dielectric constant and relative loss were found to have a maximum in the low frequency region which may be con-
tributed by the polar nature of NC. We confirmed the hydrophilic nature of the PVC/NC blends due to the presence of hydroxyl
groups by the goniometer technique. The thermophysical properties of the blends were measured by Lee's disc method. NC
loading in the blend system increased the thermal conductivity from 0.12 to 0.18 W/(m.K). The Shore A softness test of the
blends exhibited an 18% increase. We quantified structure, bandgap, morphology, and dielectric, surface and thermal proper-
ties as a function of NC blending. This new emerging blend may be a remedy for various engineering applications.
© 2022 Society of Industrial Chemistry.
Keywords: polyvinyl chloride; nitrocellulose; polymer blend; contact angle; surface energy; thermal conductivity
raw material. The nitration of natural cellulose from cotton linter are widely available. The unique features of NC combined with
or wood pulp produces NC by cooking, bleaching, washing, dry- PVC will open up new opportunities for advanced polymer blends
ing and other processes, which have a wide range of characteris- with unique physicochemical properties that have never been
tics and applications.9 Sulfuric acid is the best additive to the explored and reported before. Qualitative and quantitative ana-
nitrating mixture and delivers a great result, according to the ideal lyses of NC blends were examined by spectral, microscope, sur-
circumstances of cellulose nitration.10 The manufacturing face and thermal conductivity investigation.
methods of NC are different for different applications. The utilisa-
tion of NC is highly dependent on its nitrogen content; for exam-
ple, NC with a nitrogen content of 10.7%–12.3% is used in LITERATURE SURVEY OF PVC DERIVED
coatings and printing inks,11 while 12.6%–13.5% of nitrogen con- POLYMER BLENDS
tent is used as an explosive for gun propellants. It was first devel- Polymers exhibit interesting electrical and conductive properties
oped for use in explosives and propellants which is still one of the correlated to the structure of the polymer system. These proper-
most important markets for materials today.12 Generally, 14.14% ties may be optimised by modification of the pristine polymer sys-
is the highest concentration of nitrogen in NC when all three tem. Modification can be achieved by loading a filler, forming a
hydroxyl groups of the glucose units of cellulose are replaced with nanocomposite or blending two or more polymer systems.20 Var-
NO2. But experimentally, the maximum nitrogen content cannot ious roots or alternative methods can be used to achieve the
exceed 13.8%. If the nitrogen content exceeds this then the repul- desired chemical moieties. Polymer blends have different physical
sion forces of electronegative groups found on base rings and chemical properties depending on their structure and com-
decrease compound stability.13 Mohamed et al. reviewed the position suitable for the desired applications. Recently reported
properties and various applications of nitrogen based organic PVC polymer blends and the choice of proposed properties with
frameworks. Nitrogen doping demonstrated the mesoporous a literature survey are tabulated in Table 1.
nature of the block copolymer system.14
In addition to cotton fibres, NC and refined NC can be produced
from cellulose fibres, bamboo fibres, bagasse fibres and cellulose EXPERIMENTAL DETAILS
derived from other stalk plants.15 The cotton rod, Eulaliopsis Materials
binata, bagasse and other plant extracts were investigated and PVC polymer granules with molecular weight 233 000 g mol−1
refined into cellulose to make a thin paper.16 It can be used in used for preparation were supplied by Technovinyl Polymers
smokeless gunpowder NC products after nitration treatment. It Ltd, Mumbai (Maharashtra), India, with tensile strength of
has also been utilised for a variety of coating applications, includ- 22.8 MPa, volume resistivity 8 × 1014 Ω cm−1 and specific gravity
ing coating components, stabilisers, coating membranes, paints, 1.38 (± 0.03). A high molecular weight PVC polymer system is
lacquers, varnishes for wood, paper metal, inks for package print- deployable across a broad temperature range.31–33 NC of HM
ing, and celluloid printing. It is versatile and efficient in a variety of 10/25 grade was supplied by GRN Cellulose PVT Ltd, Ramnagar,
fields in medicine, including water filtration, power generation, Chandauli (Maharashtra), India, in cotton form with high nitrogen
catalysis coatings.17 Recently various reports showed the applica- content and medium viscosity grade. The solvent THF of AR
tion of NC and derived blends as a propellant due to its explosive grade with molecular weight 72.11 was procured from S.D. Fine-
nature. Liu C et al. prepared graphene oxide/NC membrane and Chemicals Ltd, Mumbai (Maharashtra), India, and used as is.
further, they used as as solid propellant micro thruster by using
laser ignition combustion treatment.18 Touidjine et al. prepared Preparation of PVC/NC blends
polyurethane/NC blends and further proved their suitable appli- PVC/NC blends obtained as a function of varying NC wt% were
cation as solid propellants.19 With this motivation, we selected prepared by the mix solution method. Initially, PVC and NC were
NC for polymer blending with the PVC system. dissolved in THF separately (by constant stirring at 900 rpm for 4
This research aims to prepare a new polymer blend from two and 2 h respectively at room temperature, 30 °C) to obtain com-
extensively used thermoplastics PVC and NC by the solution cast- plete dissolution. The mixed solution of PVC/NC was poured into
ing method. PVC and NC are both employed in a variety of fields a glass Petri dish. Further, to obtain blend samples the solution
since they are considered long lasting, inexpensive, air stable, and was kept at room temperature for 10 h as shown in Fig. 1. The
polymer blend sample obtained was used for further characterisa- a diameter of 10 mm and a thickness of 50–60 μm of the polymer
tion. Figures 2(a) and 2(b) show the 2D and 3D schemes of the blend was kept in a fixture.
proposed model of the blend samples. Sample configuration
details are tabulated in Table 2. Surface contact angle
A contact angle goniometer (DMe-211 Plus, Kyowa Interface Sci-
ence Co. Ltd) was used to measure the contact angle of the PVC
CHARACTERIZATION TECHNIQUES and PVC/NC blends by using different probe liquids (water, form-
Fourier transform infrared spectroscopy (FTIR) analysis amide, ethylene glycol, diiodomethane) and pouring 2.5 μL of liq-
The FTIR spectra of PVC/NC samples were determined in the uid onto the blend surface. A computer-controlled camera
region 4000–400 cm−1 using a Jasco FTIR spectrophotometer captured the liquid droplet contact angle data automatically.
6600 (Jasco FT/IR-6600). An appropriate PVC/NC blend was vali- Total five trials were taken, and the mean values were used to plot
dated with its fingerprint region. a graph.
Figure 2. Proposed model of PVC/NC polymer blends: (a) 2D view; (b) 3D view.
Beyond 20 wt% of NC samples become stickier and it is challenging to where D is the crystallite size, K is the Debye constant (K = 0.9), ⊗
get free standing film. is the X-ray wavelength (⊗ = 1.5406 Å), ⊔ is the peak angle and ⊎ is
the full width at half maximum. Evaluation of the positions and
shapes of diffraction peaks provides information about the inter-
with a small percentage of crystalline structure and is therefore planar spacing (d) and crystallinity (in percentage) of polymer
referred to as semicrystalline. On other hand, NC has a semicrys- blends. The interplanar spacing (d) was estimated using the Bragg
talline nature.35,36 Figure 3(a) shows the XRD diffractogram of equation.38 It was observed that d decreased with increased load-
pure PVC. The main diffraction peaks are observed at 2⊔ = 29.5°, ing of NC corresponding to a decrease in the number of PVC
25.1° and 39.63° of PVC which is in good agreement with recent chains packed together. Furthermore, the decreased crystallite
reports.28 The broad diffraction peak obtained at 2⊔ = 20.3° corre- size and crystallinity were confirmed by XRD data using the dif-
sponding to the amorphous phase of NC (shown in Fig. 3(b)) is fraction Eva software. Crystallite size and crystallinity were
quite similar to NC fibre.37 In the case of PVC/NC blends the peaks observed to be in the range of 42–23 nm and 70%–60% respec-
were shifted towards lower 2⊔, as shown in Fig. 3(c). It can be tively. A small crystallite size and decreased crystallinity may be
clearly seen that peaks at 2⊔ = 48.20°, 43.34°, 39.48°, 29.65° and beneficial for improvement in the micro hardness property for
25.04° shifted to 2⊔ = 44.64°, 40.43°, 36.97°, 27.80° and 21.98° the development of coating materials. It exhibited a smooth sur-
respectively. Moreover, the intensity of peaks observed at face texture.39 Calculated values of the interplanar spacing and
2⊔ = 11.15°, 13°, 14.81°, 36.22° was found to be decreased in crystallinity are summarised in Table 3.
4
Figure 3. XRD pattern of (a) pure PVC, (b) pure NC and (c) PVC/NC blends.
Figure 4. FTIR spectra for (a) pure PVC, (b) pure NC and (c) 95%/5%, 90%/10%, 85%/15% and 80%/20% (d) IR band in 500-1500 cm−1 wavenumber PVC/
NC polymer blends.
determined by optical absorption studies on pure PVC and PVC/ PVC and PVC/NC as the NC loading increases from 5% to 20%,
NC polymer blends. as shown in Fig. 5(c).
The energy gap is obtained by using the Tauc plot, fitting the The values of both the direct and indirect bandgaps decrease as
linear part of the curve and finding the intersection of the straight NC concentrations rise, as shown in the discrete plot in Fig. 5(d).
line with the hν axis.45 A variation in optical bandgap was This decrease implies the creation of charge transfer complexes
obtained for different loadings of NC. The bandgap was calcu- in the polymer blend, which could lead to defects in the polymeric
lated using the following mathematical expression referred to in matrices.
the literature. The localised states in the optical bandgap are caused by these
imperfections. When NC concentrations in the polymer matrix are
⊍hν=Aðhν-EgÞn raised, the overlaps cause the energy bandgap to decrease. Fur-
thermore, as the optical gap values drop, the degree of disorder
where ⊍ is a constant, ‘hν’ is the photon energy and ‘Eg’ is the increases (due to the amorphous nature of the produced films)
optical band gap of the semiconductor and ‘n’ is index related or local crosslinking occurs inside the amorphous phase of the
to the density of states for the energy band. mix.46
Figures 5(b) shows the direct bandgap of pure PVC and PVC/
NC polymer blends estimated using a plot of (⊍hν)2 with pho- SEM of the PVC/NC blend
ton energy hν. For pure PVC the direct bandgap lies at SEM was used to precisely explore the interaction between PVC/
3.14 eV while on adding NC it is found to decrease from 3.14 NC polymer blends. At smaller loadings of NC, it reveals good
to 2.94 eV. Similarly, the indirect bandgap was also calculated dimensional homogeneity and a uniform distribution of the pores
using the Tauc plot of (⊍hν)1/2 with photon energy hν. How- in PVC/NC. A small crater has formed on the surface of PVC/NC
ever, the indirect bandgap varies from 2.71 to 2.21 eV for pure attributed to solvent evaporation during blend formation. As a
6
Figure 5. (a) UV–visible absorption (b) direct band gap (c) indirect band gap and (d) relation curve between direct and indirect band gap of pure PVC and
PVC/NC polymer blends.
7
Figure 6. SEM micrographs of (a) 95%/5% and (b) 80%/20% PVC/NC blends.
Figure 7. Pore size of PVC/NC blends. Dielectric loss of the polymer PVC/NC blend
Dielectric loss is a measurement of electromagnetic energy dissi-
pation in a material. Figures 10(a)–10(e) show tan ⊐ versus fre-
Dielectric constant of the PVC/NC blend quency at different temperatures. For PVC tan ⊐ is observed to
A dielectric study is a versatile approach that is commonly used to be very high, ca 10. The maximum value of tan ⊐ for PVC/NC is
investigate the ionic and molecular interactions that occur within ca 6 (200 °C, 10 Hz) and it decreased further to ca 2.4 as NC load-
polymer blends, polymer composite materials. Polymer based ing increased. It is clear from the plot that tan ⊐ is high in the lower
dielectric materials are used as potentially promising alternatives frequency region and decreased for higher frequency. The
to commonly used inorganic and ceramic derived dielectric mate- charges and polar groups in the polymer blend may vibrate at
rials due to their appealing properties including greater flexibility; lower frequencies. Heat is generated through the polar torque
simple, cost-effective processing feasibility; chemical stability; and when ions overcome the resistance they face during each oscilla-
readily changeable character. With this motivation, the study of tion. This may cause a decrease in dielectric loss.24 In addition to
electrical ion exchange in dielectric properties is reported, which this effect, the oscillating dipoles and charges have a phase lag
was investigated in the present work in the frequency range about the frequency of the applied voltage. Decreased dielectric
10 Hz to 10 MHz. Figures 9(a)–9(e) illustrate plots of the dielectric loss of PVC/NC blend may enhance the electrical conductivity,
constant (εr) of (a) PVC, with a loading of (b) 5% NC, (c) 10% NC, (d) and this may lead to applications in various electronic domains.
15% NC and (e) 20% NC.48 The dielectric constant and dielectric
loss were calculated using the formulae referred to in the litera- Contact angle study of PVC/NC blend
ture.49 For PVC the dielectric constant obtained is ca 4. The maxi- For many years, contact angle measurement has been used to
mum value of the dielectric constant for PVC/NC (90%/10%) blend analyse surface wettability and roughness. It aids in the compre-
is ca 17 at 200 °C, 10 Hz. It was observed from the plot that the hension of material compatibility. Wettability is essential in the
trend of εr decreases with increase in frequency. This is because, preparation of polymer blends. We employed sessile droplets in
at low frequencies, mobile ions will have enough time to diffuse this study for contact angle measurement. Figure 11(a) shows
and migrate under the influence of the applied electric field; as contact angle values for PVC and the PVC/NC polymer blend with
a result, the charge increases in the interface region. Ions are respect to four different probe liquids (water, formamide, ethyl-
unable to be transported to the external circuit due to the block- ene glycol, diiodomethane). We observed a decreased contact
ing stainless steel electrodes. A greater εr observed in the low fre- angle for the PVC/NC blends with respect to the four liquids. This
quency domain is due to space charge effects coming from the may be due to hydroxyl groups and polar groups present in the
8
Figure 8. EDX analysis spectrum of (a) 95%/5% and (b) 80%/20% PVC/NC blends.
Figure 9. Dielectric constant of (a) pure PVC and (b) 95%/5%, (c) 90%/10%, (d) 85%/15%, (e) 80%/20% PVC/NC blends, as a function of NC (wt%)
blending.
PVC/NC blend. Hydroxyl groups show affinity towards the liquid, shown in Fig. 11(b). The rise in SE of the modified samples over
which results in improved hydrophilicity of the PVC/NC polymer the pure sample was accompanied by a decrease in contact angle.
blend over the pristine PVC sample.
Furthermore, the SE for the prepared blend sample was also
measured. For the SE measurement a proper choice of liquid is Thermal conductivity of the PVC/NC blend
very important. Liquids with γ lv ≤ γ sv become flat on a solid sur- The thermal conductivity k of a solid substance is used to deter-
face immediately. Because of this, such liquids cannot be used mine its heat transmission characteristics. It is a measure of a sub-
to determine the contact angle.30 The Owens–Wendt model was stance's ability to transfer heat by conduction through a medium.
used to estimate the SE for solid surfaces, including dispersive Thermal conductivity is measured by using various techniques.
and polar components. Diiodomethane and water were used as We used Lee's disc method and adopted the process used in pre-
the dispersive and polar components respectively for measure- vious reports.51,52 It is a quick, easy approach and a cost-effective
ment of the SE. The SE components for PVC and the PVC/NC blend method to figure out the k of materials of low thermal conductiv-
were calculated using the equations described in previous ity compared to other methods.51 Figure 12(a) shows Lee's disc
reports.50 The contact angles of water and diiodomethane on apparatus for the purpose of calculating heat conductivity using
the blend surface were measured for calculations of SE. The readily available parts. Figure 12(b) shows a heat transfer model
results showed an increased SE for the PVC/NC blend compared for pure PVC and PVC/NC blend material. The thermal conductiv-
to pristine PVC with respect to decreased contact angles, as ity k was calculated using the mathematical equation
9
Figure 10. Dielectric loss of (a) pure PVC and (b) 95%/5%, (c) 90%/10%, (d) 85%/15%, (e) 80%/20% PVC/NC blends, as a function of NC (wt%) blending.
Figure 11. (a) Contact angle of PVC/NC blend as a function of NC loading (wt%). (b) Relation curve between surface energy and contact angle of the PVC/
NC blends.
Figure 12. (a) Lee's disc apparatus. (b) Heat transfer model for PVC and the PVC/NC blends.
Figure 13. (a) Thermal conductivity of the PVC/NC blend as a function of NC loading (wt%). (b) Relation curve between thermal conductivity and specific
heat of PVC/NC blends.
situations. ⊍ increased as the mean free path increased due to shows increased absorption capacity for the PVC/NC blend com-
increased NC loading, as shown in the curve of Fig. 13(a). The spe- pared to PVC. The Cp curve of the PVC/NC blend is illustrated in
cific heat capacity (Cp) is an evaluation of a material's capacity to Fig. 13(b). The results show the importance of dispersion and suit-
absorb heat from its environment. It signifies the quantity of able compatibility between the NC and PVC blend. This enhanced
11
energy needed to produce a temperature rise. The increased Cp thermal conductivity, diffusivity and specific heat capacity is
ACKNOWLEDGEMENTS
The authors would like to gratefully acknowledge the Institute of
Chemical Technology Mumbai Marathwada Jalna for providing a
doctoral fellowship. Research scholar Pratibha S. Jadhav is grateful
to the Vellore Institute of Technology, Vellore (India), for providing
the SEM characterisation facility.
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