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Nanomaterials 2020, 10, 454 4 of 13 was confirmed by UV-visible spectroscopy (UV-Vis; UV-1700, Shimadzu, Japan) within the wavelength range with 200–700 nm. The morphology of GO sheets and the size of AgNPs were evaluated by transmission electron microscopy (TEM; JEM-1200EX, Beijing, China). The lattice spacing of AgNP was determined by high-resolution transmission electron microscopy (HRTEM). The XRD pattern was obtained with X-ray diffraction (XRD) using a Bruker D8 Advance diffractometer (Bruker, Beijng, China). 3. Result and Discussion Characterization of Composites and Membranes The images of GO and GO/AgNPs composite solution and membrane were shown in Supplementary Figures S2 and S3, respectively. FTIR spectra of GO and GO/AgNPs composite is shown in Figure 1a. The peak at 3430 cm−1 corresponds to −OH stretching band. The peaks at 1740, 1610, 1230 and 1050 cm−1 are assigned to C=O stretching vibration, C=C vibration, C−O−C stretching and C−O stretching, which indicate successful synthesis of GO. Some prominent peaks shifted after AgNPs modification. Because of the strong interaction between Ag+ ions and carboxyl groups on the edges of GO sheets, the intensity of −OH decreases sharply, and both the intensity and peak position of C=O group changed, as shown in the FTIR spectra of GO/AgNPs composite. The intensity and peak position of C−O−C and C−O groups also changed, which indicates that the vast oxygen-containing functional groups contribute to the proper decoration of AgNPs on GO sheets. Compare to GO, GO/AgNPs composite have obvious change in peak position and intensity, which shows composite does not produce new chemical bonds, but due to the electrostatic adsorption. Figure 1b shows Raman spectra of GO and GO/AgNP composites. Comparing to GO, the D and G band obviously enhanced after AgNP modification, because of surface enhanced Raman scattering from the forceful local electromagnetic fields of AgNPs along with the plasmon resonance. The intensity ratio of GO/AgNPs composite (ID/IG = 1.02) is also higher than that of GO (ID/IG = 0.92), indicating a decrease in the average crystallite size of GO−AgNPs composite, due to more defects in graphene composite material after AgNPs modification. [27] The degree of disorder decreased because of the average crystallite size of GO-AgNPs composite decreasing. ID/IG ratio is inversely proportional to the average crystallite size and the degree of disorder. A TEM image of GO is shown in Figure 2a. The TEM image and size distribution of three types of GO/AgNP composites are shown in Figure 2b–d,f–h. The sizes of AgNPs loaded on the three types of GO/AgNP composites are 8 nm, 20 nm and 33 nm, respectively, as shown in Figure 2f–h, which is consistent with TEM image (Figure 2b–d). Therefore, we called them GO-8, GO-20 and GO-33. An HRTEM image of AgNPs loaded on a GO sheet is shown in Figure 2e. The inter-planar distance between the fringes is 0.24 nm, which is corresponds to the (200) lattice plane of Ag. Figure 3a shows UV-Vis absorption spectra of GO and GO/AgNP composites. As shown in Figure 3a, there is a maximum at 230 nm (indicating the electronic π−π* transitions of aromatic C−C bonds) and a shoulder at about 306 nm (assigned to the n−π* transitions of C−O bonds) in the UV-Vis spectra of GO. After AgNP modification of GO, the UV-Vis spectra of GO-8, GO-20 and GO-33 all have a characteristic peak of AgNP at 398 nm, 406 nm, and 410 nm. The characteristic peak range of AgNP is between 398 nm and 420 nm, and shifts to larger wavelength with increasing size of AgNP, which is consistent with TEM image (Figure 2b–d) and size distribution (Figure 2f–h).The XRD patterns of GO and three types of GO/AgNP composites are shown in Figure 3b. The characteristic peak of GO can be observed at 2θ = 11.02◦. The peaks at 2θ = 38.16◦, 44.28◦, 64.28◦, and 77.42◦ are assigned to the (111), (200), (220), and (311) reflection of Ag.PDF Image | Graphene Oxide Nanofiltration Membranes Silver Nanoparticles
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