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treatment time of t = 120 s, the treated liquid surface heated up by about 5 K. This temperature increase does not explain the fast and controlled silver nanoparticle synthesis. iii) The stabilizer sodium citrate is not capable of acting as a reducing agent under the experimental conditions. Therefore, the plasma activation of the pure stabilizer solution and Nasnuobmsaeteqriualesn20t20a,d10d,i5t5io5n to the silver nitrate solution also did not lead to the formation of6soifl1v2er nanoparticles. 3.2. Form and Position of the Plasmon Resonance Peak 3.2. Form and Position of the Plasmon Resonance Peak In Figure 4, the progression of the spectral absorbance of the samples S1 and S4 up to a plasma In Figure 4, the progression of the spectral absorbance of the samples S1 and S4 up to a plasma treatment time t = 120 s is shown. The typical silver nanoparticle plasmon resonance peak above treatment time t = 120 s is shown. The typical silver nanoparticle plasmon resonance peak above 400 400 nm increases with the treatment time t. The position of the plasmon resonance peak serves as a nm increases with the treatment time t. The position of the plasmon resonance peak serves as a benchmark of the nanoparticle size [41]. For the stock solution S1, the maximum wavelength of the benchmark of the nanoparticle size [41]. For the stock solution S1, the maximum wavelength of the plasmon resonance peak is roughly at 412 nm. In S4, the resonance peak is approximately at 423 nm plasmon resonance peak is roughly at 412 nm. In S4, the resonance peak is approximately at 423 nm and, thus, larger nanoparticles were created [41]. and, thus, larger nanoparticles were created [41]. A further peak appears around 255 nm, which is a signal of the solution [10]. This peak also A further peak appears around 255 nm, which is a signal of the solution [10]. This peak also increases with the plasma treatment time t, which is due to the change in the chemical composition increases with the plasma treatment time t, which is due to the change in the chemical composition inside the solution. In this wavelength range, nitrites NO −,−nitrates NO − −[42,43], and hydrogen 23 inside the solution. In this wavelength range, nitrites NO2 , nitrates NO3 [42,43], and hydrogen peroxideHO [44]cancontributetothesignal,whichindicatestheirformationinthestocksolution 22 peroxide H2O2 [44] can contribute to the signal, which indicates their formation in the stock solution during the plasma treatment. during the plasma treatment. (a) (b) Figure 4. Absorbance spectra over treatment time t, displayed every 8 s up to a maximum treatment timFiegoufret =4.1A2b0ssofrobran(ac)eSs1paenctdra(bo)vSe4r.treatment time t, displayed every 8 s up to a maximum treatment time of t = 120 s for (a) S1 and (b) S4. As the plasma treatment time t increases, the plasmon resonance signal becomes broader. A suitable explanation could be a broadening caused by a larger particle size distribution [27], aggregation As the plasma treatment time t increases, the plasmon resonance signal becomes broader. A processes of the created nanoparticles [45], or changes in particle shape [30]. The signal broadening suitable explanation could be a broadening caused by a larger particle size distribution [27], aggregation processes of the created nanoparticles [45], or changes in particle shape [30]. The signal depends on the composition of the stock solution and the ratio between silver and citrate ions, broadening depends on the composition of the stock solution and the ratio between silver and citrate respectively. The stock solution S4 shifts to the reddish wavelength range, mainly attributed to agglomeration processes between the nanoparticles, caused by insufficient stabilization due to the ions, respectively. The stock solution S4 shifts to the reddish wavelength range, mainly attributed to high ratio of silver ions to citrate ions of 7:5 [45,46]. agglomeration processes between the nanoparticles, caused by insufficient stabilization due to the high ratio of silver ions to citrate ions of 7:5 [45,46]. Imaging via transmission electron microscopy (TEM) was used to check the possible aggregation, particle size distribution, and particle shape. TEM images of different stock solutions containing nanoparticles after different treatment times t with corresponding particle size histograms and UV/VIS absorption spectra are illustrated in Figure 5. It is recognizable that at a treatment time of t = 10 s, the particles in stock solution S2 are spherical and the majority of the particles are in the size range of dparticle ≤ 2 nm. In addition, some spherical nanoparticles with particle diameters of dparticle ≤ 10 nm, which possess a higher optical activity [47], are already present. The characteristics of the UV/VIS absorption signal after t = 10 s are narrow and show a defined shape; these characteristics also symbolize the observed attributes of the formed nanoparticles. With longer treatment times t, the silver nuclei and small nanoparticles grew to larger silver nanoparticles [48,49] in the stock solution S2. At a treatment time of t = 30 s, particle–particle unions, staple faults [50], twinned crystals [48], and also non-spherical nanoparticles appeared. Crystallization processes leading to the resulting crystal structure of silver [48] cause the change in particle shape. After a treatment time of t = 60 s for stock solution S4, particle–particle unions, non-spherical nanoparticles, and staple faults occur more frequently. Particles with a maximum particle diameter of dparticle ≈ 130PDF Image | Formation Kinematics of Plasma-Generated Silver Nanoparticles
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