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Polymers 2020, 12, 1155 3 of 16 2. Materials and Methods 2.1. Materials The chemicals used in this study, including extra pure graphite powder (>99.5%), potassium permanganate (>99%), silver nitrate, and hydrogen peroxide (30%), were supplied from Merck, while the hydrazine hydrate (HH) (80%) was provided by Loa Chemi. The monomers (i.e., styrene (S) and methyl methacrylate (MMA)) and the initiator (i.e., benzoyl peroxide (BP)) used in this study were obtained from Acros Chemical Co. and BDH Chemicals Ltd., Saudi Arbia respectively. All of the chemicals were analytical grade and used without any further purification. 2.2. Preparation of RGO/AgNPs The GO was synthesized via the Hummers and Hoffman method reported in previous work [11]. Initially, the GO (400 mg) was suspended in 25 mL of H2O and sonicated for 30 min, followed by the addition of silver nitrate solution (80 mg, 20 wt. %) and further mixing for 30 min. The solution was then placed inside a conventional microwave oven (Kenwood MW740) after adding 40 μL of the reducing agent hydrazine hydrate (HH), and the operating conditions were set to full power (i.e., 900 W) with an on and off pulse of 10 and 20 s, respectively, for 1.2 min [16]. Following this, centrifugation was carried out using a Centurion Scientific Ltd. centrifuge operated at 5000 rpm for 15 min and the solid was dried overnight at 80 ◦C. AgNPs were prepared via a similar procedure, in the absence of RGO and GO. 2.3. Preparation of RGO/AgNPs-(PS-PMMA) A mixture of PS/PMMA (1:1 wt. %), RGO/AgNPs (i.e., 2 wt. %), and BP initiator (i.e., 5 wt. %) was sonicated for 1 h. The mixture was then kept at 60 ◦C for 20 h to promote in situ free radical polymerization. Next, the product was washed several times using excess methanol and hot water. Finally, the prepared RGO/AgNPs-(PS-PMMA) nanocomposite was dried in an oven at 80 ◦C overnight. For comparison, a neat PS-PMMA copolymer was also prepared via a similar procedure in the absence of RGO and GO. 2.4. Preparation of R-(GO-(PS-PMMA)-AgNPs by MWI A mixture of PS/PMMA (1:1 wt. %), GO (i.e., 2 wt. %), and BP (i.e., 5 wt. %) was sonicated for 1 h, and then polymerized via the in situ bulk polymerization method, as described in the previous section, to produce GO/PS-PMMA nanocomposites. Then, 40 μL HH in the presence of 0.08 g silver nitrate was added to the GO/PS-PMMA (i.e., 0.40 g) nanocomposite and sonicated for 1 h, followed by MWI reduction. 2.5. Material Characterization and Testing The chemical structure properties of the prepared nanocomposites were studied using FT-IR (Thermo Scientific Nicolet-iS10) spectra between the ranges of 4000 and 500 cm−1. Additionally, X-ray diffraction (XRD, Philips-Holland, PW 1729) with Cu radiation was used to investigate the properties of the nanocomposites between 2θ of 5 and 100◦. The X-ray photoelectron spectrum (XPS, SPECS GmbH) measurements of the nanocomposites were taken after degassing under vacuum inside the load lock for 16 h. In addition, the Raman spectra of the prepared nanocomposite were measured using a Bruker Equinox 55 FT-IR spectrometer equipped with a FRA106/S FT-Raman module and a liquid nitrogen cooled Ge detector using a 1064 nm line of an Nd:YAG laser with an output laser power of 200 mW. The microstructural morphology of the prepared nanocomposites was investigated using a scanning electron microscope (SEM, FEI Quanta 200, FEI, Hillsboro, OR, USA). The nanocomposites were coated with gold via a sputtering system (Polaron E6100, Bio-Rad, UK). For high-resolution transmission electron microscopy (HR-TEM) images, JEOL JSM-2100F, Japan, was used withPDF Image | Microwave Irradiation Synthesis Silver Nanoparticle
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