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surface; (d,f) SEM graphs of RCF and CANF0.04 cross‐section. The crystal lattice of the obtained cellulose films was type II (Figure 5), and more silver crystal peaks appeared in the spectrum. The average particle size of the Ag‐NPs in CANF0.01 to CANF0.08 was increased by calculation, whereas the cellulose crystallinity was declined. There is a correlation Polymers 2020, 12, 440 8 of 15 between the two tendencies: the increase of Ag‐NPs concentration in film fabrication process caused the nanosilver particles more easily to agglomerate, and the average particle size increased. In more uniform filling Ag-NPs within cellulose structures may affect the cellulose crystallization ability, addition, more uniform filling Ag‐NPs within cellulose structures may affect the cellulose resulting in a decrease in cellulose crystallinity of the films. crystallization ability, resulting in a decrease in cellulose crystallinity of the films. Cellulose peaks Ag peaks Grain size: 36.02 nm 30.62 nm 28.39 nm 18.45 nm - nm - nm Crystallinity: 55.10% 59.21% 70.46% 74.35% 78.88% 79.27% CANF0.08 CANF0.04 CANF0.02 CANF0.01 CANF0.005 RCF TypeII Intensity / a.u. (001) (-101) (-201) 10 20 30 40 50 60 2 Theta / degree Figure 5. XRD patterns of composite ffiilms. The full XPS scan results of RCF and CANF were shown in Figure 6a. The C1s and O1s peaks The full XPS scan results of RCF and CANF0..04 were shown in Figure 6a. The C1s and O1s peaks were obvious in the figure. The weak peak appeared CANF in the binding energy range of 380–360 were obvious in the figure. The weak peak appeared CAN0.F040.04 in the binding energy range of 380– was the Ag3d peak. Note that there were no obvious S and Si peaks in the spectrum indicated the less 360 was the Ag3d peak. Note that there were no obvious S and Si peaks in the spectrum indicated the MPTS content on the film surface. This occurred because only a small amount (1% typical of filler less MPTS content on the film surface. This occurred because only a small amount (1% typical of filler mass) of MPTS could completely coat the nanoparticles, and most of them may be removed during the mass) of MPTS could completely coat the nanoparticles, and most of them may be removed during immersion process. The oxygen and carbon atomic ratios (O/C) of RCF and CANF surface were the immersion process. The oxygen and carbon atomic ratios (O/C) of RCF and CANF0.0.044 surface were 0.522 and 0.558, respectively, which were close to the O/C values of common wood fibers [39]. The O/C 0.522 and 0.558, respectively, which were close to the O/C values of common wood fibers [39]. The value of RCF was slightly lower than CANF , which indicated that the addition of Ag-NPs may O/C value of RCF was slightly lower than CAN0.0F40.04, which indicated that the addition of Ag‐NPs may introduce some oxygen-rich components on the film surface. The C1 (C–C, C–H), C2 (C–O, C=N), and introduce some oxygen‐rich components on the film surface. The C1 (C–C, C–H), C2 (C–O, C=N), C3 (N–C–O, C=O) content obtained from C1s spectrum of RCF were close to the CANF (Figure 6c,d), and C3 (N–C–O, C=O) content obtained from C1s spectrum of RCF were close to the C0.A04NF0.04 (Figure showing that the addition of Ag-NPs has little effect on the C-containing components of the film surface. 6c,d), showing that the addition of Ag‐NPs has little effect on the C‐containing components of the C4 (–O–C=O) content of CANF was higher may attribute to a carboxylic acid structure produced film surface. C4 (–O–C=O) conte0n.0t4of CANF0.04 was higher may attribute to a carboxylic acid structure duringthereductionofAg+withDMAc+similartoAg+withN,N-dim+ethylformamide[34,36].TheAg produced during the reduction of Ag with DMAc similar to Ag with N,N‐dimethylformamide content on the surface of CANF calculated from the Ag3d peaks was 0.86% (Figure 6b), whereas [34,36]. The Ag content on the su0r.0f4ace of CANF0.04 calculated from the Ag3d peaks was 0.86% (Figure no obvious Ag3d peaks appeared on the RCF surface, suggesting that the Ag-NPs were successfully 6b), whereas no obvious Ag3d peaks appeared on the RCF surface, suggesting that the Ag‐NPs were loaded on the cellulose film surface. successfully loaded on the cellulose film surface. The lithium element content of RCF and CANF summarized by ICP test were 0.252 mg/g and The lithium element content of RCF and CANF0.04 summarized by ICP test were 0.252 mg/g and 0.241 mg/g, respectively, whereas the lithium content of 1 g film was close to that of 1 L of soft water, 0.241 mg/g, respectively, whereas the lithium content of 1 g film was close to that of 1 L of soft water, revealing that the low LiCl content in CANF may not harmful. The GC-MS test results (Figure A1) revealing that the low LiCl content in CANF may not harmful. The GC‐MS test results (Figure A1) showed the DMAc residue in RCF and CANF was much lower than 100 μg/g, which limited the showed the DMAc residue in RCF and CANF0.04 was much lower than 100 μg/g, which limited the OEKO-TEX Standard 100. This can be attributed to the easier removal of the residual solvent in the OEKO‐TEX Standard 100. This can be attributed to the easier removal of the residual solvent in the relatively thin film (the average thickness of the films was approximately 20–40 mm). Therefore, the relatively thin film (the average thickness of the films was approximately 20–40 mm). Therefore, the immersing process could effectively remove the most residual Li/DMAc system of the film, reducing immersing process could effectively remove the most residual Li/DMAc system of the film, reducing potential harm to organic beings. potential harm to organic beings. The surface and cross section of RCF and CANF0.04 were dense (Figure 4c–f), and the transmittance of composite films exceeded 70% (Figure 7), corresponding to the reported high transparency cellulose-based composite films [40], indicating that the Ag-NPs-MPTS had prominent affinity with cellulose. As the Ag-NPs content increased, the more opaque Ag-NPs were dispersed uniformly in the film, resulting in a decline in film transparency. The decrease in cellulose crystallinity was also a cause of light transmittance decline. In addition, the large number of Ag-NPs promotes the increase of surface roughness of CANF, which lead to the light scattering ability enhanced, thereby the film haze was increased. The slowing trend of light transmittance and haze changed with the increase of Ag-NPs suggested the addition of too much Ag-NPs may cause a weaker effect on changed the film properties.PDF Image | One-Pot Synthesis of Antibacterial Silver Nanoparticle
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