1. INTRODUCTION:

Conducting polymers have recently attracted many researchers in various scientific and technological fields due to a mixture of properties, such light weight, low cost, thermal and radiation stability, as well as excellent electrical, optical and mechanical properties [1-4].

Poly 4, 4-diaminodiphenyl sulphone (PDDS) is a new conductive polymer of the poly aniline family. It is synthesized by the chemical and electrochemical polymerization method [5]. On the other hand, PDDS is an electro-active polymer [6] used in the fields of electrochromicity as promising materials, energy storage as capacitors and a promoting agent for photo catalytic reactions [7] due to its higher conductivity, high electro activity and good solubility in organic compounds [8].

Polymer nanocomposites have been of great interest thanks to the advantages provided by the dispersion of inorganic materials at the nanometric scale in a polymer matrix [9,10]. These have several advantageous properties compared to metals and ceramics, such as their lightness, low cost, surface/volume ratio, lower size, ease of implementation, and several improved physico-chemical properties [11-13]. Polymer/clay nanocomposites have attracted a lot of attention in recent decades due to their important properties relative to polymer or conventional micro and macro composite [14]. Polymer/clay nanocomposites are prepared by incorporating layer silicate materials dispersed in a polymer matrix. Nevertheless, the nanolayers do not disperse easily in most polymers due to the incompatibility of hydrophilic silicates with the hydrophobic polymer matrix, Therefore the layered silicates must first be changed organically by adding hydrophobic agents to create the polymer-compatible clay (organic clay) [15-17]. Next, the most commonly used methods for the synthesis of polymer-claynanocomposite are the in-situ polymerization, mixing in solution and mixing in the melting state [18, 19]. The addition of clay to polymers, even at very low load, was found to enhance the physicochemical properties of polymers such mechanical, thermal, barrier properties, durability, chemical stability, flame retardation, and biodegradability [20-22]. All these properties are associated with the process used to prepare the nanocomposites and the nature of the clay [23].

In this article, the clay/polymer nanocomposites based on poly 4,4-diaminodiphenyl sulfone (PDDS) and clay modified were prepared via in-situ emulsion polymerisation method. The properties of PDDS/modified clay nanocomposite were examined by Fourier transform infrared spectroscopy (FTIR), UV-visible spectra, X-ray diffraction (XRD), Thermogravimetric analysis (TGA), the morphological properties of the hybrids were investigated by scanning electron microscopy (SEM) and their electrochemical behavior were studies by cyclic voltammetry.

2. MATERIAL AND METHODS:

2.1. Reagents:

All materials (4, 4-diaminodiphenyl sulfone (DDS), Ammonium persulfate (APS) and ammonia solution (NH₄OH)) were purchased from Aldrich and used without further purification. The raw clay was obtained from Tlemcen (Algeria).

2.2. Preparation of maghnite (mag):

The clay used in this study (named as Mag) was obtained from Tlemcen (Algeria). The raw-montmorillonite was washed with distilled water to remove impurities. Next, the Mag was crushed and sieved to obtain particles smaller than 100 microns. The activation of maghnite by sodium was performed using NaCl solution (1M) and 40g maghnite, which were mixed at room temperature for 24 hours and washed several times with distilled water to remove chloride. Then, the solid (Mag) was recovered by centrifugation, washed with plenty of water and dried at 80°C. The resulting clay is called Mag-Na.

To prepare the Mag-Ni, 5g of Mag-Na was dispersed into a 100ml nickel nitrate solution (1M) and stirred for 24h at room temperature. Next, the Mag-Ni was separated by centrifugation and washed four times with distilled water. Finally, the product was dried at 70 °C for 24h. With the same protocol, we prepared the Mag-Co using cobalt nitrate [24,25].

2.3. Preparation of the hybrid nanocomposite:

The polymerization was carried out in a 100ml flask, ice bath and magnetic stirrer. Firstly, The Mag (0.1g) and the monomer 4,4-diaminodiphenyl sulphone (DDS) (4 mmol) were dissolved in 10ml of HCl (0.1M) and stirred for 30 min. Then ammonium persulphate (APS) solution (0.022M) was added dropwise within 15 minutes and the reaction was carried out at (0-5°C) for 24 h. Finally the product was filtered, washed with distilled water and dried at room temperature for 48h [26,27].

2.4. Characterization section:

UV spectrafor poly (4, 4-diaminodiphenyl sulphone) nanocomposite were characterized by a Septrum sp-uv 200 S and were performed in a quartz cuvette using the N, N-diméthylformamide (DMF) solution. Fourier transform infrared spectra were recorded using Cary 630 FT-IR equipment. The Philips analytical X- ray diffractometer instrument was utilized to record the X-ray diffraction of the hybrid nanocomposite. The Scanning Electron Microscopy (SEM) analysis was employed using a tabletop microscope, model (TM-1000). Thermogravimetric analyses (TGA) were performed from room temperature to 800°C using a Du Pont thermogravimetric analyzer under N₂ and O₂ atmosphere at a heating rate of 10°C/min.

The electrochemical behaviour of PDDS and PDDS-Mag nanocomposite were studied by cyclic voltammetry (CV) using a conventional three-electrode cell. The reference and counter electrodes were produced by a plate of platinum and Ag/AgCl. The sulphuric acid H₂SO₄ (0.1 M) was used as the electrolyte. All tests were performed at 50mV/s. For the preparation of the working electrode, a quantity of PDDS nanocomposite material was treated in the solvent N, N-diméthylformamide (DMF), then poured onto platinum discs and dried to remove the solvent.

3 RESULTS AND DISCUSSION:

3.1. FTIR spectral behavior of nanocomposite:

The infrared spectra of the Mag-Co, Mag-Ni, PDDS, PDDS-Mag-Co and PDDS-Mag-Ni are shown in Fig. 1 The spectrum of the Mag-Co and Mag-Ni showed the peaks at 3620-3628, 1005-1012 and 794-796 cm^-1, which are attributed to the O-H stretching of the hydroxyl group, Si-O stretching vibration in the tetrahedral layer and Al-OH bonds vibration, respectively [28,29].

In the FTIR spectrum (Fig. 1) of PDDS, PDDS-Mag-Co and PDDS-Mag-Ni, The peaks observed at 3598 cm^-1 and 1642 cm^-1are assigned to the N-H stretching and bending vibrations of the imino group [30,31]. The bands at around 1592 cm^-1 and 1496 cm^-1may be attributed to the C=C stretching of quinoid and benzenoid rings, respectively. The bands at approximately 1156 cm^-1 and 1299 cm^-1 can be assigned to stretching vibrations of sulfone S=O, symmetric, and asymmetric group shows. In addition, the clay band is observed in 1008 cm^-1 and 1012 cm^-1 for the vibration of Si-O bonds for PDDS-Mag-Co and PDDS-Mag-Ni, respectively, which can be indicated the formation of nanocomposite [32,33]. The detailed peak positions with their mode of vibration for PDDS and their nanocomposites are presented in Table 1.

Table 1: FTIR spectra peak position and their mode of vibration for PDDS, PDDS-Mag-Co and PDDS-Mag-Ni.

Type of nancomposites	Wave number (cm⁻¹)	Mode of vibration
PDDS	3366	N–H: stretching
	1642	N–H: bending
	1592	C=C: stretching
	1297	S=O: stretching
	1105	C–H: in-plane bending
	834	C–H out-of-plane bending
	693	C=C bending vibration
	570	S=O bending
PDDS-Mag-Co	3365	N–H: stretching
	1640	N–H: bending
	1591	C=C: stretching
	1296	S=O: stretching
	1103	C–H: in-plane bending
	1008	Si-O: stretching
	833	C–H out-of-plane bending
	695	C=C bending vibration
PDDS-Mag-Ni	3366	N–H: stretching
	1641	N–H: bending
	1592	C=C: stretching
	1297	S=O: stretching
	1101	C–H: in-plane bending
	1012	Si-O: stretching
	835	C–H out-of-plane bending
	697	C=C bending vibration

Fig. 1: FTIR spectra of Mag-Co, Mag-Ni, PDDS, PDDS-Mag-Co and PDDS-Mag-Ni nancomposites.

3. 2 UV-vis Spectra of nanocomposites:

The UV-visible spectra of PDDS-Mag-Co and PDDS-Mag-Ni recorded for samples of these polymers dissolved in DMF at 230-800 nm are shown in Fig. 2. The band in the range of 240 nm was observed for both polymers associated with the π-π* transition of the aromatic heterocyclic. A peak with the approximate λ_max value of 350 nm for all these polymers can be attributed to a π-π* transition of conjugated benzenoid rings [34-36].

Fig. 2: UV-vis spectra of PDDS-Mag-Co and PDDS-Mag-Ni nanocomposites.

3.3. XRD studies of nanocomposites:

Fig. 3 and Table 2 show the XRD patterns of the sample Mag, Mag-Co, Mag-Ni, PDDS, PDDS-Mag-Co and PDDS-Mag-Ni, respectively. The peaks in the region’s 20-27° 2θ were observed in all samples of clay, which can be attributed to the amorphous silica remaining in montmorillonite. The peak at 2θ values of 6.25° for Mag (d₀₀₁=14.13 Å) is shifted to 5.51° for Mag-Ni (d₀₀₁=16.02 Å) and 5.05° for Mag-Co (d₀₀₁=17.48 Å). The shifting to a lower angles and the increase of the d-value signifies the intercalation of the inorganic cation (nickel or cobalt) in the clay. The PDDS shows an amorphous background XRD pattern, which reveals the lower crystalline nature of the polymer.

In the PDDS-Mag-Co nanocomposites, three sharp peaks are clearly observed at 21.88°, 23.52° and 25.75° that correspond to the d-spacing of 4.05, 3.77, and 3.45 Å. These peaks suggested to the crystal structure of PDDS nanocomposite. Moreover, the disappearance of the peak at 5.51° of Mag-Ni in the case of PDDS-Mag-Ni indicated the formation of exfoliated clay structures. Furthermore, the peaks at 22.92°, 24.71° and 26.94° may be attributed to the high crystalline nature of PDDS-Mag-Ni nanocomposite. [34,37,38]. Finally, the diameter of the nanoparticles (crystallite sizes) was calculated by using Scherrer formula as

kλ

D= ------------

β.Cos θ

Where D is crystallite sizes, k is Scherrer constant, was considered as 0.9 in this work. λ is the X-ray wavelength, β is the line broadening value at half of the maximum intensity (FWHM), which is expressed as Δ2θ in radians, and θ is the Bragg angle. The calculated crystallite sizes of the samples PDDS, PDDS-Mag-Co and PDDS-Mag-Ni are 30.17, 21.38 and 20.58nm respectively.

Table 2: Peak maximum and d-spacing of the sample Mag, Mag-Ni, Mag-Co, PDDS-Mag-Ni and PDDS-Mag-Co.

Samples	Peak maximum, 2θ max (º)	Basal spacing, d(001) (Å)
Mag	6.25	14.13
Mag-Ni	5.51	16.02
Mag-Co	5.05	17.48
PDDS-Mag-Co	//	Exfoliated
PDDS-Mag-Ni	//	Exfoliated

Fig. 3: XRD diffraction patterns of Mag, Mag-Co, Mag-Ni, PDDS, PDDS-Mag-Co and PDDS-Mag-Ni.

3.4. SEM analysis:

The SEM photograph of PDDS, PDDS-Mag-Co and PDDS-Mag-Ni are shown in Fig. 4. The SEM image of PDDS (Fig. 4a) presents an organized and self-assembled structure with small cavities. In contrast, the morphology of PDDS-Mag-Co (Fig. 4b) and PDDS-Mag-Ni (Fig.4c) have the granular irregular structures with particles of smaller and bigger sizes. Finally, the significance difference of morphology between PDDS and PDDS-Mag nanocomposites can be attributed to the dispersion of the PDDS between the clay layers [39, 40].

Fig. 4: SEM images of PDDS (a), PDDS-Mag-Co (b) and PDDS-Mag-Ni (c).

3.5. Electrochemical response of nanocomposites:

Fig. 5 shows the cyclic voltammograms (CVs) of the PDDS, PDDS-Mag-Co and PDDS-Mag-Ni nanocomposite. A low-current CV curve is obtained for pure PDDS. However, the nanocomposite PDDS-Mag shows large oxidation and reduction peaks in the CV curve, which is similar to that of pure PDDS. Moreover, the anodic and cathodic peak potential values for the two nanocomposite are respectively at Epa ~540mV and Epc ~320mV. The main difference between PDDS-Mag-Co and PDDS-Mag-Ni is the shifting of the peak current which in the PDD-Mag-Ni appear to higher current values. Finally, these results indicate to the conductivity of all nanocomposite is higher compared to PDDS due to the conducting network formation of Mag-Ni or Mag-Co in the polymeric matrices [41,42].

Fig. 5: Cyclic voltammetric response of PDDS, PDDS-Mag-Co and PDDS-Mag-Ni nanocomposites at scan rate 50 mV s⁻¹ in 0.1M H₂SO₄ medium.

3.6. Thermal stability characteristics:

The thermogravimetric curves (TGA) plots of Mag- Co, Mag-Ni, PDDS, PDDS-Mag-Co and PDDS-Mag-Ni are presented in Fig. 6. TGA curves for Mag-Co and Mag-Ni show an initial weight loss approximately 5 wt% in the temperature range of 50°C to 200°C, which is assigned to the removal of adsorbed water and interlayer water. A second weight loss in the temperature range of 200–800°C which is associated to the elimination of the hydroxyl groups located in the interlayers of the clay [33,43]. In the case of PDDS, 2% weight loss at temperature of 50°C to 137°C is due to the removal of water molecules from the polymer matrix, the weight loss above 20% within the temperature range of 137–422°C can be assigned to the pyrolysis of the polymer. The weight loss observed from 422°C onwards, which can be indicated to the degradation of polymer chain. Moreover, the PDDS-Mag-Co and PDDS-Mag-Ni nanocomposites present three discrete stages in TGA curves such as removal of humidity at 140°C, elimination of the acid dopant bound and low molecular weight oligomers in the temperature range of 140-450°C and the degradation of polymer molecules at temperature higher than 450°C. Finally, the TGA curves show the thermal improvement in the case of PDDS-Mag nanocomposites, which can be confirmed the incorporation of the clay materials into the polymer matrix [44-47].

Fig. 6: TGA of Mag-Co, Mag-Ni, PDDS, PDDS-Mag-Co and PDDS-Mag-Ni obtained in nitrogen atmosphere at heating rate of 10 °C/min.

4. CONCLUSIONS:

This paper describes for the first time the synthesis of PDDS-clay modified via in-situ emulsion polymerisation method using ammonium persulfate (APS) as an oxidizing agent. FTIR, Uv-visible, DRX and SEM results revealed the formation of exfoliated clay structures in PDDS chain. The TGA curves of PDDS-clay modified present the good thermal stability and cyclic voltammetric studies showed the better reversible redox behaviour for PDDS-clay modified, which is indicated to these nanocomposites can be used as an electrode material for supercapacitors applications.

5. ACKNOWLEDGEMENTS:

This work was supported by the Directorate General of Scientific Research and Technological Development (DGRSDT) of Algeria.

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Received on 05.09.2020 Modified on 29.10.2020

Asian J. Research Chem. 2021; 14(1):73-78.

DOI: 10.5958/0974-4150.2021.00012.2