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The colour of the precursor solution changed to yellow after a few minutes of the plasma treatment, indicating the formation of the nanoparticles. All the samples present the characteristic surface plasmon resonance peak of silver nanoparticles (Figure 2). A slight but significant peak was observable for 1 min of plasma exposure, but this later became more prominent. The width of the Nanomaterials 2020, 10, 874 4 of 10 each plasmon is related to the size distribution of the nanoparticles. The 3‐min, 5‐min and 7‐min samples produced peaks at 369 nm, 394 nm and 396 nm, respectively. The 1‐min and 10‐min samples have their surface plasmon peaks at 404 nm and 416 nm, respectively. Since equal volumes of samples same concentration of precursor, the peak height of the absorbance can be directly proportional to reacted using the same concentration of precursor, the peak height of the absorbance can be directly the concentration of the synthesised nanoparticles. The nanoparticle concentration increases until it proportional to the concentration of the synthesised nanoparticles. The nanoparticle concentration reaches 5 min and then there is a slight decrease at 7 min. At 10-min plasma exposure, the decrease is increases until it reaches 5 min and then there is a slight decrease at 7 min. At 10‐min plasma more prominent and the plasmon resonance peak is red shifted, which can be attributed to polydisperse exposure, the decrease is more prominent and the plasmon resonance peak is red shifted, which can distribution of silver nanoparticles [18]. be attributed to polydisperse distribution of silver nanoparticles [18]. Figure2. Ultraviolet‐-visible(UV-‐Vis)sspeeccttrraooffththeesilsvilevrenranaonpoapratirctlieclsesysnytnhtehseiseisdedonodniffdeirffeenrtepntlasma pexlapsomsuarextpiomseusre(lteifmt)e;ssi(zleftd);istirziebudtiisotrnibouftAiognnoafnAogpanratnicolpesarmticelaesumreedasbuyrethdebDyythneamDiycnLaimghictLSicgahttering Scattering (DLS) method technique for different plasma exposure times (right). (DLS) method technique for different plasma exposure times (right). Unlikemiiccrroossccooppicictetcehcnhinqiuqeuse,sD,LDSLmSemaseuarseusrethsetheydhryodryondaymniacmdicamdieatemreotferthoeftheortheteicoarletical sphere (rather than the physical size) that diffuses with the same speed as the measured nanoparticle. sphere (rather than the physical size) that diffuses with the same speed as the measured nanoparticle. This is determined by the stabilisers adsorbed on to the nanoparticle, and the solvation shell also This is determined by the stabilisers adsorbed on to the nanoparticle, and the solvation shell also moves along with the particle [19]. Therefore, the size measured using the DLS technique is slightly moves along with the particle [19]. Therefore, the size measured using the DLS technique is slightly larger than the results obtained by the microscopic techniques. Moreover, DLS measurements are larger than the results obtained by the microscopic techniques. Moreover, DLS measurements are hardly possible on smaller particles in a polydisperse solution [20]. According to the DLS data hardly possible on smaller particles in a polydisperse solution [20]. According to the DLS data obtained obtained from the samples (Table 1 and Figure 2 right), there is a decrease in nanoparticle size with from the samples (Table 1 and Figure 2 right), there is a decrease in nanoparticle size with an increase an increase in plasma exposure time. The largest average diameter of 20.06 nm is observed at 3 min in plasma exposure time. The largest average diameter of 20.06 nm is observed at 3 min of plasma of plasma treatment and it was then observed that the diameter decreases gradually with an increase treatment and it was then observed that the diameter decreases gradually with an increase in treatment in treatment time. The lowest average particle diameter of 9.99 nm was observed at 10 min of plasma time. The lowest average particle diameter of 9.99 nm was observed at 10 min of plasma exposure. exposure. This is an important finding since sub 10‐nm silver nanoparticles has been proven to be This is an important finding since sub 10-nm silver nanoparticles has been proven to be extremely extremely effective on antibacterial activity. Since DLS measures the hydrodynamic diameter of the effective on antibacterial activity. Since DLS measures the hydrodynamic diameter of the nanoparticles, nanoparticles, the actual size of the resulting particles can be much smaller than 9.99 nm, which will the actual size of the resulting particles can be much smaller than 9.99 nm, which will be far more be far more effective on disinfection processes. Additionally, more than 90% of the volume effective on disinfection processes. Additionally, more than 90% of the volume percentage can be found percentage can be found within the peak area, indicating a narrow distribution of nanoparticles within the peak area, indicating a narrow distribution of nanoparticles formed during the experiment. formed during the experiment. Table 1. Variation of DLS size values on different exposure times of cold plasma. Table 1. Variation of DLS size values on different exposure times of cold plasma. Plasma Exposure (min) % Volume 20.06 90.9 Standard DSteavniadtaiordn Plasma Exposure (min) DLS (nm) % Volume 3 5 7 20.06 90.9 5.543 DLS (nm) Deviation 3 5 7 10 5.543 16.16 95.9 15.2716.16 92.2 95.9 3.746 9.99 98.4 3.405 15.27 92.2 4.322 4.3223.746 The morphology of the silver nanoparticles has been analysed using TEM. Figure 3a–d show the images of the particles synthesised under 3, 5, 7 and 10 min of cold plasma exposure. The shape is near spherical and the average diameters of the nanoparticles were 17.9 ± 8.9, 14.3 ± 1.6, 10.6 ± 2.3, and 5.4 ± 1.4 nm, respectively. The High-resolution transmission electron microscopy (HRTEM) images of the silver nanoparticles synthesised under different plasma exposure times are shown in the Figure 3e–g.PDF Image | Bactericidal Silver Nanoparticles by Plasma Processing
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