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Nanomaterials 2020, 10, 555 4 of 12 Table 1. Temperatures and electron density inside the plasma discharge. Parameter OH-rotational temperature N2-rotational temperature N2-vibrational temperature Electron density 2.4. Investigation of Formation Kinetics Value 669 ± 134 K 820 ± 50 K 3017 ± 742 K 3.8 × 1021 ± 2.4 × 1021 m−3 To determine the kinetics of nanoparticle synthesis using an atmospheric pressure plasma, UV/VIS absorption spectra were recorded in situ during the plasma treatment. For those measurements, the UV/VIS spectrometer AvaSpec-UL3648 (Avantes, Apeldoorn, The Netherlands) with a deuterium halogen lamp AvaLight-DH-S (Avantes, Apeldoorn, The Netherlands) was used. The spectra were recorded every 0.5 s with an integration time of 1.5 ms and averaged over 50 spectra using the software AvaSoft 8.9 (Avantes, Apeldoorn, The Netherlands). The plasma treatment and, thus, the nanoparticle synthesis took place in a UV cuvette for durations of 5, 10, 20, 30, 60, and 120 s. For the analysis, the spectra were smoothed by a Savitsky–Golay filter and, afterward, evaluated using peak analysis via Origin 2018 (OriginLab Corporation, Northampton, MA, USA). In order to obtain nanoparticle samples suitable for transmission electron microscopy (TEM), grids (100 mesh hexagonal copper covered with a formvar film) were incubated with droplets of different nanoparticle solutions. Those droplets were dried by carefully absorbing the excess liquid with a piece of filter paper. Then, the nanoparticles were imaged with a LEO912 transmission electron microscope (Carl Zeiss Microscopy, Oberkochen, Germany) by using an on-axis 2k CCD camera (TRS, Moorenweis, Germany). The particle sizes were measured automatically with the software ImageJ 1.52p [24]. Furthermore, the pH-value of the solutions was measured using pH-meter FiveGo F2 with an InLab Flex-Micro electrode (Mettler Toledo, Columbus, OH, USA). In addition, the sample temperature was determined immediately after switching off the plasma with the thermal imaging camera TiS (Fluke Corporation, Everett, WA, USA). 3. Results and Discussion The coloration of the stock solutions after different plasma treatment times is shown in Figure 3. A yellow tint is typical for silver nanoparticles [25] and changes over the plasma treatment time and concentration of the stock solution. For the highly concentrated S4, the coloration shifts to reddish. The optical properties of silver nanoparticles in solution are dependent on particle size [26–28], particle material [25,29], particle shape [30,31], particle coating [32,33], particle stabilization [34], and particle Nanomaterials 2020, 10, 555 environment [30,35]. (a) 5 of 13 (b) (d) (c) Figure 3. Coloration comparison of the stock solutions (a) S1, (b) S2, (c) S3, and (d) S4 after plasma Figure 3. Coloration comparison of the stock solutions (a) S1, (b) S2, (c) S3, and (d) S4 after plasma treatmtreantmt iennUt inVUcuVvceutvtetsteosvoevrearnanasacsecennddiing plasmattrreeaatmtmenetntimtime teritsirnisginfrgomfrolemft tloefrtigtohtr(i5g,h1t0,(52,0,10, 20, 30, 603,0,1620, s1)2.0 s). 3.1. Synthesis Pathways In order to gain more detailed insights into the formation of silver nanoparticles, some process-determining kinetic parameters and the synthesis routes are explained below. The coloration of the stock solution by the plasma is an indication of the formation of silver nanoparticles [25]. The generated electrons, ions, radicals, and electromagnetic fields provided at thePDF Image | Formation Kinematics of Plasma-Generated Silver Nanoparticles
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