This paper reports a study on conductive textiles prepared by chemical oxidative polymerization of anizidine using ammonium persulfate as an oxidant. A two-step process is adopted. The morphology of treated and control cotton were studied by SEM. The study has shown the polymer granules on the treated fabric.  Polyanizidine presented into treated cotton was confirmed by ATR-FTIR and WAXD.  The thermal properties were studied by ATG and DSC confirming polymer deposition into cotton fabric.   

Ayoub, H.S.

Issaoui, C.

Sadok, R.

English

Revues Scientifiques Marocaines

 I. Chefia & al. / Mor. J. Chem. 4 N°2 (2016) 561-566  561       Physicochemical characterization of a polyanizidine coated cotton fabric  I. Chefia, H.S. Ayoub, R. Sadok   Laboratory of Interfaces and Advanced Materials, Monastir University FSM, 5000, Monastir, Tunisia   *Corresponding author: issaoui_chefia@yahoo.fr   Received  01 Mai 2016, Revised 05 May 2016, Accepted 08 May 2016  Abstract   This paper reports a study on conductive textiles prepared by chemical oxidative polymerization of anizidine using ammonium per sulfate as an oxidant. A two-step process is adopted. The morphology of treated and control cotton were studied by SEM. The study has shown the polymer granules on the treated fabric.  Polyanizidine presented into treated cotton was confirmed by ATR-FTIR and WAXD.  The thermal properties were studied by TGA and DSC confirming polymer deposition into cotton fabric.   Keywords: coated, cotton, morphology, thermal properties.  1. Introduction  On very different markets from those of aesthetics and fashion, technical textiles have objective features and essential performance. They conquered almost all industrial sectors from electronics to aerospace, civil engineering to construction and automotive to medical. We must therefore confront multidisciplinary knowledge to bring out the technical textiles of the future. The conductive textile may be produced by coating with conductive materials, such as metals, metal, carbon black, carbon nanotubes and conductive polymers. These fibers are known as conductive coated fibers [1-4]. With coating processes, not only higher conductivities may be achieved, but also the mechanical properties of the fibers can be improved. These properties depend not only on the type of conductive materials but also the coating technique used. For metal coatings, sputtering and vacuum deposition are the most used methods [5-6]. High conductivities similar to those of metal (10 S / cm) can be achieved with these methods. However, the high cost, rigidity and high weight limit their application in the field of textile. Carbon black, carbon nano-tubes and conductive polymers can be applied in a thin layer on a fiber by jet printing or in situ polymerization [4, 7-10]. The thin films provided by coating have a relatively high conductivity, flexibility and elasticity [10]. Carbon black and carbon nanotubes have a high conductivity, exceptional environmental stability and a low weight. However, their use is very limited due to their toxicities. Conductive polymers [9, 11, 12] are reasonable candidates for textile functionalization. However, difficulties in processing and poor adhesion to the substrate can be met. Using appropriate coating techniques and compatible substrates, these problems can be minimized. [13]. Because of technological progress in the textile industry, a variety of textile fibers with exceptional mechanical properties have been developed. The coating of the high-strength fibers with conductive polymers may form a multifonctionality. Attempts have already been made on textile substrates  I. Chefia & al. / Mor. J. Chem. 4 N°2 (2016) 561-566  562   such as viscose, PET, lyocell, nylon, cotton, using conductive polymers such as poly (pyrrole), poly (aniline) and PEDOT [10, 14-18]. Several features should be introduced into the clothes. Most of them were done by the incorporation of electronic and metal devices to perform different tasks; to connect, transfer and communicate data [19]. Using this technology, many products were marketed primarily for medical apparel, sportswear and protective clothing [20-23]. But the integration of sensors, power sources, or electronic components in clothing reduces comfort, makes the process more complex, increases the weight of the garment, and also increases the cost of the product. [24] However, due to promising developments in science and technology of organic materials, it is possible nowadays to incorporate conductive polymers in the structure. These polymers can meet all sorts of features- namely the detection, power generator production and storage of energy in the intelligent and interactive systems. These devices can be obtained either by coating textile materials by conductive polymers or by mixing thermoplastic materials with conductive components. In this study, a conducting textile has been elaborated by a two steps process. The fabric was firstly impregnated in the monomer’s solution than in the oxidant one. So, the polymerization will took place inside cotton fabric.  The coating textile was characterized by ATR-FTIR and WAXD analysis to confirm conducting polymer presence. The thermal properties show an increasing in thermal stability of treated fabric.           2. Materials and methods  2.1. Materials and chemicals Cotton woven fabric of 132 g / m2 weight, 0.19 mm thickness, 15 ends per cm, and 15 picks per cm was chosen as a substrate for this study. The chemicals used were   Ammonium persulfate (NH4) 2S2O8 brand: Sigma Aldrich and purity of 99.7%.  Anizidine derived from aniline C7H9NO chemical formula (FLUKA) All these chemicals were of laboratory grade and they were used as received.  2.2. Preparation of electro-conductive fabric The method we have used to coat textile is the two-step method. Two baths monomer and oxidant are prepared:  12.3g (0.100mol) of anizidine was dissolved in a 1 M HCl 100mL solution and maintained under magnetic stirring.  28.5 g (0.125mol) of (NH4)2S2O8 was dissolved in 100 ml of an aqueous solution of HCl 1M well stirred.   These two solutions are kept at 0° C. Each sample was impregnated in the monomer bath for 45 minutes. Then, the sample is impregnated in the oxidant bath for 45 minutes. This process is repeated three times. At the end, the samples are soaked in a 1 M HCl solution; then removed, washed and finally dried.  2.3. Conductivity measurement   Electrical conductivity was measured by an electrometer witch measure the electrical resistance R using the equation 1. Where  R : electrical resistance (Ω);  e : Thik (cm);  d : Distance between tw electrodes (cm) and re : ray of electrode (cm) and Conductivity was calculated as σ = 1/ρ   I. Chefia & al. / Mor. J. Chem. 4 N°2 (2016) 561-566  563                   (eq1)  3. Results and Discussions  3.1. Morphology study   Coating cotton morphology had been studied and figure1 show SEM micrograph of untreated and treated cotton fabric. The fabric is actually saturated and even inside at the level of fiber and this is visible in the SEM micrograph. Cotton textiles are very hygroscopic. So, they absorb the oxidant which will be located inside blocked between the sites of the fibers and pores. After exposure of the fabric to the monomer, there will be polymerization within these pores and therefore the polymer is deposited around the fabric. The untreated fabric shows a clear surface with twisted fibers characterizing the cotton fiber. The polymerization of polyanizidine on cotton fabrics takes place by the diffusion of polymer within the fiber and the deposit on the surface of the fibers and interstices in the fabric. SEM micrograph shows the polymer granules on the treated fabric. These granules are also thrown into the polymerization bath in the form of dark green to black powder. Therefore, the granular structure is the deposit polyanizidine on the surface.     (a) (b) (c)                                                                       Figure1.  SEM micrographs of PANIZ-CT fabrics (a- untreated, b–treated with a magnification of 200, c–treated with a magnification of 1500  3.2. Conductivity study  Conductivity study was done in our previously study [25] and we retched a conductivity below 0.04 Scm-1.   3.3. ATR-FTIR analysis The Fourier transforms infrared spectroscopy (FTIR) of the polymer, the reference cotton and the treated cotton was conducted. We present in Figure2 the FT-IR spectra of the polymer (paniz), control cotton and treated cotton. The superposition of the spectra of the polymer, control cotton and treated cotton shows the existence of characteristic bands of paniz and control cotton in the spectrum of the treated cotton. In particular, for control cotton, the broad band centered about 1000 cm-1 corresponds to the frequencies of the C-O-C. This band shifts to 1100 cm -1 in the case of the treated fabric and becomes thinner. Similarly, we note the emergence of a new band around 1200 cm-1 for the case of cotton treated which is a characteristic band of the C-N function of the polymer. In addition, we note the disappearance of the band assigned to the C-H in the case of processed cotton.  I. Chefia & al. / Mor. J. Chem. 4 N°2 (2016) 561-566  564   Two broad bands the first located around 1500 cm-1 relative to C-C bond and the second around 1600 cm -1 assigned to the C = C bond characteristic of the polymer,  were present in the spectrum of the treated fabric, which confirms the presence of the polymer in the treated fabric.  1600 1400 1200 1000 800 600 C-O-C)Transmittance (%)  Wave number (cm-1) control cotton treated cotton PANIZsC-O-C)asC-O-C)C-N)C-H) ArC-C) ArvinC=C)(c)(b)(a)def(C-H) def (O-H)  Figure2. ATR-FTIR spectra of control, treated cotton and PANIZ  3.4. The WAXD analysis Patterns for the control cotton (b) and the cotton / paniz (a) are shown in figure3. The diffraction pattern of X-ray untreated cotton shows maxima at 2Ɵ equal to 14.9 and 22.77. The peak maxima cotton / paniz are located at 2Ɵ = 15.3 and 22.97, and values are slightly shifted to the upper side. From this, we can conclude that paniz molecules were distributed in the cotton fabric. Furthermore, additional peaks appear at 37.79 and 44.02 corresponding to the crystals of pure paniz. This reveals the presence of paniz in the cotton fabric 0 10 20 30 40 50 600200400600800100012001400160018002000intensity (a,u)20 (deg) cotton control treated cotton(a)(b) Figure3. XRD spectra of control and treated cotton   I. Chefia & al. / Mor. J. Chem. 4 N°2 (2016) 561-566  565   3.5. Thermal studies The thermal properties of treated and untreated cotton were analyzed under ambient conditions by thermal gravimetric analysis (TGA). Analyzes were carried out between room temperature and 600 ° C with a heating rate of 10 ° C / min. The two thermograms are shown in figure4. Thermo gravimetric analysis reveals the effect of the polymer on the thermal stability of treated fabric. In the case of the treated fabric (a) thermo-degradation starts around 284 ° C with a weight loss of 68%. This reduction in weight loss is mainly due to the increased rigidity of the polymer fixed on the fabric. 0 100 200 300 400 500 600020406080100% Mass Temperature (°C) treated cotton(a) control cotton(b)81,32 %68,22%296°C(b)284°C(a)  Figure4. TGA curve of control and treated cotton  The thermal properties of treated and untreated cotton are studied under ambient conditions by differential scanning calorimetric (DSC). The study was carried out between room temperature and 300 ° C with a heating rate o-f 10 ° C / min. The three thermograms were shown in figure5, the treated cotton result on the superposition of the two thermograms of polymer and control cotton. This proves the existence of the polymer in the treated cotton.   50 100 150 200 250 300ExoHeat Flow  (mW)Temperature (°C)  PANIZ (c) Treated cotton (b) Control cotton (c)(c)(b)(a) Figure 5. DSC thermo grams of PANIZ, control and treated cotton   I. Chefia & al. / Mor. J. Chem. 4 N°2 (2016) 561-566  566   4. Conclusion We succeeded in this paper to develop a conductive textile using two step methods by impregnating the substrate in successively in oxidant and monomer bath. We studied the thermal and chemical properties of the treated fabric (cotton / polyanizidine). In conclusion, a conductive textile has been successfully prepared by covalently grafting PANIZ onto a cotton fabric substrate   References [1] D. Kincal, A. Kumar, A. D. Child, J. Reynolds, Synth. Met., 92 (1998) 53-56. [2] D. Zabetakis, M. Dinderman, P.,Schoen, , Adv. Mater., 17 (2005) 734-738. [3] P. Xue, and X.M. Tao, J. Appl. Polym. Sci., 98 (2005) 1844-1854. [4] D.Negru, C.T Buda, D. Avram, Fibers & Textiles in Eastern Europe., 20 (2012) 53-56. [5] D. Meoli, T. May-Plumlee, Journal of Textile and Apparel, Technology and Management., 2 (2002). [6] A.k. Sen, Coated Textiles Principles and Applications. J. Damewood, Editor 2001, Technomic Publishing Company, Inc. [7] H. Dirk, G. Mac. D.  Alan, M. S.  David, E. 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Physicochemical characterization of a polyanizidine coated cotton fabric

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Physicochemical characterization of a polyanizidine coated cotton fabric

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