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Polymers 2019, 11, 2000 6 of 21 to identify crystalline silver in the composite structures, and collected on a Rigaku SmartLab X-ray diffractometer (Tokyo, Japan) with Cu Kα radiation (λ = 1.542 Å), operating at 60 kV and 60 mA, over the 15–90◦ 2θ angle range at a step size of 0.01. Nanoparticle size and size distribution of the particles have an impact on the agglomeration behaviour of the precursor mixtures and were measured at a pH of ~7, on a Brookhaven Instruments Corporation ZetaPlus Potential Analyzer (Holtsville, NY, USA). 2.6. Wash Fastness of Composite Textiles (AATCC TM61-2001; ISO105-C10:2006) Wash durability was evaluated at 40 ◦C with 4 g/500mL ECE Phosphate Reference Detergent (SDC Type 3) for 30 min, with 10 steel balls (each weighing ~0.9 g, with a diameter of 0.7 mm), in a Launder-O-meter (SDL Atlas, Hong Kong, China) [80]. Four accelerated wash cycles (equivalent to 12 conventional laundering cycles) were conducted on the polyviscose composites (further cycles were not possible due to substrate damage resulting from polyviscose sensitivity to laundering and drying). Antimicrobial testing and chemical characterisation of sample swatches was carried out before and after wash fastness testing. 2.7. NP Leachant Testing Using Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES) The content of Ag-leaching in the substrates was determined using an Agilent Technologies 5100 ICP-OES (Santa Clara, CA, USA). Following sample preparation, polyviscose substrates of either Ag or Ag-rGO coating, (1.0 × 1.5 × 0.15 cm, ~15–18 mg) were immersed in 20 mL saline solution (0.85%), stirring at 100 rpm for 3 h at 40 ◦C, and the concentration of silver released into solution measured. Silver concentration was determined against a calibration curve prepared using a Sigma Aldrich ICP silver element standard solution. The calibration curve method utilises an internal standard to minimise errors caused by instrumental drift and reduces chemical matrix effects [18,81,82]. A blank and a three-point calibration curve were generated using concentrations of 1.0, 5.0, and 10.0 ppm of the silver element standard, and a linear fit chosen in the on-board software. Sample dilution was not required since the ppm levels detected were under the calibration limits. For quantification, the calibration curve had a correlation coefficient R2 > 0.995, with the mid-point of the calibration curve well within 1% of the theoretical concentration. The calibration and textile samples were analysed in 0.5M HNO3(aq). 3. Results and Discussion 3.1. Nanoparticle-Impregnated Polyviscose Substrate Synthesis In this study, well-dispersed silver nanoparticles (AgNP) were immobilised over a reduced graphene oxide (rGO) support via a facile two-step wet-impregnation method at room temperature, which leads to well-defined “plasmonic-graphene hybrids” over the surface of non-woven, polyviscose substrate supports. This correlates with past reports on alternative hard supports [83–85]. The process is substrate-mediated. Thus, rather than use a surfactant, the rough, porous surface of the textile fabric substrate comprising a multitude of functional groups and micropores acts as the micro-reactors and nucleation points as well as size-controlling agents that constrain the size of AgNP agglomerations, which allow an effective upper band on cluster sizes [73]. The functional groups (e.g., carboxyl) are coordinated such that the silver cations directly attach via electrostatic interactions, which facilitates the co-reduction process, after having been converted to borohydride functional species [59,60]. Consequently, a stable GO-Ag nanocomposite forms. The Ag+/GO composite is reduced to Ag0 species, simultaneously with the reduction of adjacent GO to rGO [86]. While a range of reducing agent concentrations (1–200 mmol) were utilised in this project, the data presented in the main body of this article relates to the 200 mmol samples. The full datasets are available in the SI. Varying NaBH4(aq) concentration offers a remarkably powerful but simple route for controlled, increasingly mono-disperse and isotropic NP growth/incorporation and composite formation, with all other factors being equal. Therefore, this removes the trouble of a broader multi-component precursorPDF Image | Antimicrobial from Silver-Graphene Coated Medical Textiles
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