Supplementary Information for. Silver Nanoparticles Embedded Anti-microbial Paints Based on Vegetable Oil
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1 Supplementary Information for Silver Nanoparticles Embedded Anti-microbial Paints Based on Vegetable Oil Ashavani Kumar #, Praveen Kumar Vemula #, Pulickel M. Ajayan, George John * Department of Chemistry, The City College of New York, and The Graduate School and University Center of The City University of New York, New York, New York Department of Materials Science and Engineering, Rensselaer Polytechnic Institute Troy, New York Current address: Department of Mechanical Engineering and Material Science, Rice University, Houston, Texas * Corresponding author john@sci.ccny.cuny.edu # authors are equally contributed to the paper Index Figure S1. TEM images of AgNPs and GNPs and UV/spectra Figure S2. XPS graphs and analysis of Ag + ion presence Figure S3. Summary of EDX experiments Figure S4. Time dependent UV of AgNPs in oils Figure S5. Images of NPs containing coatings on various surfaces Figure S6. Schematic representation of NPs-paint interaction with bacteria Table S1. Summary of antibacterial efficiency of AgNPs containing paints Characterization of poly(cardanyl acrylate) page no.. S2.. S3.. S4.. S5.. S6 S7.. S7.S8 S1
2 Figure S1 TEM images of AgNP and GNPs in paints. TEM images of a and b, AgNPs-oil films and c and d, GNPs-oil films. Metal nanoparticles embedded films were cut into slices (microtomed) with 100 nm thickness and few microns in length which were placed on cupper grid and subjected to TEM. e, Absorption spectra of in situ synthesized GNPs in drying oil. Average particle of GNPs size is nm. S2
3 Figure S2 Summary of XPS experiments. AgNP containing paint was coated on silicon substrate and analyzed by X-ray photoemission spectroscopy. Lower and higher binding energy component of Ag3d core-level spectra. Binding energy of Ag3d core level spectra shows the presence of silver ions (Ag + ) and metallic silver (Ag 0 ) in the paints. XPS analysis details. In order to quantify the ratio of Ag + to Ag 0, we carried out X-ray photoemission spectroscopy. The Ag nanoparticles-oil medium is quite homogeneous so chemical composition does not change from surface to bulk. A solution-cast film of silver nanoparticles -oil was formed on Si(111) substrates and analyzed by XPS. A general scan spectrum of the film at room temperature showed the prominently presence of C 1s, O 1s and Ag 3d core levels with no evidence of impurities. The film was sufficiently thick and, therefore, no signal was measured from the substrate (Si 2p core level). Fig. S2 shows the Ag 3d core level spectra recorded from the Ag-oil film formed by the drop-coating technique. The Ag 3d spectrum could be resolved into a two spin-orbit pair (splitting ~6 ev) with a 3d5/2 binding energy (BE) of and ev (the core levels were aligned with respect to the adventitious C 1s BE of 285 ev). This BE corresponds to that of Ag(0) and Ag(I) state of silver and are in good agreement with the reported value 1. The area occupied by peak is proportional to amount of silver present in different oxidation state in the samples. The ratio of area occupied of Ag (0) to Ag(I) peak is 7.5:1 indicate the relative ratio of metallic silver and silver ion present in the sample. 1. Kumar, A. et al. Phase transfer of silver nanoparticles from aqueous to organic solutions using fatty amine molecules. J. Colloid Interface Sci. 264, (2003). S3
4 Figure S3 Summary of EDX experiments. SEM images of oils films with a, AgNPs and b, GNPs. Spot analysis of metal nanoparticles [c, AgNPs and d, GNPs) contained oil films using energy-dispersive X-ray diffraction (EDX). Green and red spectra correspond to NPs and blue spectra correspond to the background where no metal nanoparticles present. Black arrows show the characteristic peaks to the metals, i.e., peaks at kev (Kα) and kev (M) of silver c, and gold d, respectively. S4
5 Figure S4 Absorption spectra of AgNPs in drying oils. Absorption spectra of AgNPs synthesized in drying oils in presence and absence of autoxidation promoting catalyst (Fe 2+ ). Absorption spectra of with without catalyst (equal concentrations of other components at similar conditions) recorded at different time points, importantly, initially (red and black) they are identical. In presence of free-radical formation promoting catalyst complete AgNPs formation was achieved in 2 hours, on the contrary, in the absence of catalyst it needs 6 hours for completion. In addition, both cases absorbance did not change over long period of time (12 hours) indicating the particle formation has been completed and NPs are stable in the oil media. S5
6 Figure S5 NPs containing paints on glass surface. Drawings of a smiley (left) and glass slide (right) with AgNPs-paint (yellow in color) and GNPs-paint (pink in color). These NPs containing alkyd resins can be coated on nearly on all kind of surfaces. S6
7 Figure S6 NP-paint interaction with bacteria. Schematic representation of AgNPs-paint coated on desired surface which decontaminate the bacteria when it get in contact to the bacteria. Table S1. Bactericidal activity against airborne S. aureus and E. coli of glass slides coated with AgNPs embedded vegetable drying oil (AgNPs-paint). a bactericidal efficiency, e % surface S. aureus E. coli blank glass b 0 0 glass+paint c 0 0 glass+agnps paint d nearly total nearly total a Bacterial suspensions (5 X 10 6 cells/ml) in a PBS aqueous solutions were sprayed onto surface of interest, dried in air for 5 min, placed in a Petri dish, covered with 1.5% solid growth agar, sealed, and incubated t 37 ºC overnight, and then the colonies were counted. b Commercially available glass slide (2.5 X 7.5 cm) was used as such without coating. c Glass slide was coated with vegetable drying oil (in this sample there are no AgNPs present). d Glass slide was coated with AgNPs embedded vegetable drying oils (AgNPs-paint). e Bactericidal efficiency is defined as the number of bacterial colonies/cm 2 observed following cultivation on a coated slide divided by that in the case of the corresponding non-coated slide, times 100%. All experiments were carried out at least in triplicate. S7
8 Characterization of poly(cardanyl acrylate). The number- and weight-average molecular weights of polymer was determined by a Waters Associates model 440 gel permeation chromatograph having µ-styragel column of pore size 10 5, 10 4, and 10 3 Å connected in series and UV detector. Chloroform was used as the mobile phase. The instrument was calibrated using standard samples of polystyrene. The number- and weight average molecular weights of the polymer before cross-linking as determined by GPC were 3000 and 11,000 respectively. DSC: DSC was recorded using a Mettler TA 3000 system in air at a heating rate of 5ºC/min from 30 to 200ºC. DSC curve of poly(cardanyl acrylate) shows an exotherm at ºC and a peak maxima of 132.1ºC, indicating a polymerization reaction. This might be due to cross-linking of polymer. IR: The C-H stretching vibrations of the unsaturated part of the side chain of the monomer CA was observed at 3020 cm -1, which is characteristic of disubstituted olefinic system. This is further clarified from the observation that this peak is absent in saturated analog of cardanyl acrylate where the side chain has no double bond. The double bond of acrylic moiety was observed at 1658 cm -1, and in the poly(cardanyl acrylate), the peat at 1658 cm -1 was not observed, due to the conversion of acrylic C=C to C-C, where as the peak at 3020 cm -1 did not change. This is clearly indicating that the side chain of monomer with its double bonds remains intact in the polymer and polymerization takes place only through the acrylate double bonds. 1 H-NMR: In the 1 H-NMR of cardanyl acrylate monomer the peaks were assigned for different protons (δ, ppm): 0.8 (t, CH 3 ), [m, (CH 2 )], (nr, -CH 2 -CH=CH-), (nr, -CH 2 - Ar), (t, CH 2 =CH-, -CH=CH-), (m, =CH 2 ), (m, -CH=), (m, aromatic). In the NMR spectrum of poly(cardanyl acrylate) the peak at δ = (acrylic) is not present due to polymerization through acrylate moiety and the peak at δ = for the double bonds in the side chain of the monomer remains intact after the polymerization reaction, which also supports the IR data. S8
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