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Polymers 2019, 11, 2000 7 of 21 variation [87,88]. Benefits include (i) minimal wastage of expensive precursors, (ii) ability to re-use unused precursor, (iii) a room temperature process, done in situ, which negates purification or transfer steps [89], (iv) controlled, increased, and uniform interaction of species throughout various substrate shapes, which is ideal for textiles and related soft matter. After coating, substrates underwent a color change. Due to deposition of AgNPs, the colourless substrates turned a yellowish brown. Those with rGO turned a grey-black while the Ag-rGO combinations yielded a brown-black colour. Polymers 2019, 11, 2000 7 of 21 3.2. Nanoparticle-Impregnated Composite Bonding Interactions, Materials Characterisation, 3.2. Nanoparticle-Impregnated Composite Bonding Interactions, Materials Characterisation, and Durability and Durability Testing Testing SEM images, bright-field contrast optical microscopic images of fibers as well as longitudinal SEM images, bright-field contrast optical microscopic images of fibers as well as longitudinal and cross-sectional images are presented in Figure 1. The optical microscope images indicate clear and cross-sectional images are presented in Figure 1. The optical microscope images indicate clear variations between the Ag-impregnated, rGO-impregnated, and Ag-rGO impregnated substrates. variations between the Ag-impregnated, rGO-impregnated, and Ag-rGO impregnated substrates. The darker coloured aggregates indicate the presence of additives as the result of light absorption or The darker coloured aggregates indicate the presence of additives as the result of light absorption or scatter, with the greater density of aggregates in Ag-rGO samples indicating a higher loading overall. scatter, with the greater density of aggregates in Ag-rGO samples indicating a higher loading overall. SEM images clearly display characteristic rGO lamellar sheets, which are decorated with AgNP for SEM images clearly display characteristic rGO lamellar sheets, which are decorated with AgNP for Ag-rGO samples, which shows successful loading. The images indicate fibrous surfaces decorated with Ag-rGO samples, which shows successful loading. The images indicate fibrous surfaces decorated AgwNiPthaAgglNomPeargagtleosmoefrpaotelysdoifspoelrysdeidspisetrsiebudtiisotrnisbuintisohnaspinesahnadpdeianmdedteiar,maettaecrh,aetdtatcohreGdOtosrhGeOetsh[9ee0t,9s1]. Itis[9i0m,9p1o].rtIatnitstiomnpootertathnatttpoanrtoicteletshoabtspearvrteidcleosnotbhseetrevxetdileosnurthfaecetevxitaileSEsMurfcaocmepvriaiseSEaMcolcloemctipornisoefaAg crycsotalllelicteiosnanodf ,Athgucsr,yasrtealmlituecshalnadrg, ethr uths,anartehemcurcyhstlalrlgiterstizheasnetshteimcarytesdtabllyitethseizSecshesrtriemr aetqeudabtiyonth[e92]. Scherrer equation [92]. The primarily spherical agglomerations observed in this case are also reflected The primarily spherical agglomerations observed in this case are also reflected in the UV–Vis data in the UV–Vis data where there is no observable lateral plasmon shift signal. where there is no observable lateral plasmon shift signal. Figure 1. (a) SEM images of for nanocomposite-incorporated polyviscose fibers, both (i) before laundering, Figure 1. (a) SEM images of for nanocomposite-incorporated polyviscose fibers, both i) before and (ii) after laundering, (b) Dark-field optical microscope images of nanocomposite-incorporated laundering, and ii) after laundering, (b) Dark-field optical microscope images of nanocomposite- polyviscose fibers with longitudinal microscopy images inset. incorporated polyviscose fibers with longitudinal microscopy images inset. After the laundering tests of 12 equivalent standard wash cycles, both simple visual appraisal and After the laundering tests of 12 equivalent standard wash cycles, both simple visual appraisal optical microscopy indicate that laundering causes fabric damage. This degradation takes the form of and optical microscopy indicate that laundering causes fabric damage. This degradation takes the an increasingly flattened substrate as well as some structural thinning. SEM indicates a greater degree form of an increasingly flattened substrate as well as some structural thinning. SEM indicates a of aggregation and enhanced ball-like formation observed on the samples. Post-wash, it seems that the greater degree of aggregation and enhanced ball-like formation observed on the samples. Post-wash, solely AgNP samples exhibit enhanced release, even though the metal presence is still detected and it seems that the solely AgNP samples exhibit enhanced release, even though the metal presence is observed [93]. The seemingly greater presence of AgNP on the rGO samples indicates reduced relative still detected and observed [93]. The seemingly greater presence of AgNP on the rGO samples outflow of AgNPs, i.e., higher laundering durability and binding [94,95]. indicates reduced relative outflow of AgNPs, i.e., higher laundering durability and binding [94,95]. XRD and EDS data are given in Figure 2a,b. EDS confirmed the presence of silver on polyviscose XRD and EDS data are given in Figure 2a and 2b. EDS confirmed the presence of silver on subpsotlryavteiscsousrefascuebsswtraitheasusrifganceifiscwanitthlyahsiighneifricAangt-lwyth%ighreradAign-gwdte%tecrteeadifnogrdAegte-rcGteOdfsoarmApgle-rsGtOhan forssaomlepllyesAthgaNnPfosrasmolpeleysA. PgNosPt-slamunpdlesr.iPnogs,tw-lahuilnedtehreinagm, wohuinlet tohfedaemteocutendt oAf gdedtectreedasAegs dinecarlelacsaeses, natiunralllcya,stehse, ninaittuiraalllpyr,et-hweainshitiarellparteio-wnsahshipresltaitlliohnoslhdips,stoillahloalrdgse, tdoeaglraereg.eTdhegereme.eTanhevmaleuaensvbaelucoesme become ~0.4 wt % (AgNP, from ~14.2 wt %; which is in agreement with past reports of >90% material ~0.4 wt % (AgNP, from ~14.2 wt %; which is in agreement with past reports of >90% material loss in loss in textiles) [96] versus ~8.2 wt % (Ag-rGO, from ~34.3 wt %). Thus, the presence of rGO seems to textiles) [96] versus ~8.2 wt % (Ag-rGO, from ~34.3 wt %). Thus, the presence of rGO seems to improve improve both initial loading as well as longer-term adherence to the substrate. The silver loading both initial loading as well as longer-term adherence to the substrate. The silver loading values on values on cellulosics, as obtained through the surface treatment process, are much higher than past cellulosics, as obtained through the surface treatment process, are much higher than past reports, reports, which have ranged from 0.2–2.3 wt % silver on initial textile loading [97–101]. This highlights the efficacy and potency of the surface treatment route adopted in this study. The expected XRD signals for GO/rGO, which are usually observed at ~10° and ~25° 2θ, were completely blocked by the polyviscose substrate signal [102,103]. Nevertheless, the silver incorporated samples yielded prominent peaks that were solely assigned to the well-defined crystalline FCC phase. There was no evidence of oxidation, nitridation, or any other mixed phase presence. The observed peaks atPDF Image | Antimicrobial from Silver-Graphene Coated Medical Textiles
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