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Nanomaterials 2020, 10, 376 4 of 22 2.3. Characterization Fourier transform infrared spectroscopy (FTIR), ultraviolet–visible absorption spectroscopy (UV–vis), X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, X-ray diffraction (XRD), and transmission electron microscopy (TEM) were employed to evaluate the structure and the morphology of the samples. 2.3.1. FTIR Analysis FTIR spectra of GO and GO–AgNPs were recorded on a Thermo Nicolet iS10 spectrometer (Thermo Fisher Scientific, Madison, WI, USA) equipped with an attenuated total reflectance accessory (ATR). 2.3.2. UV–vis Analysis A Perkin Elmer Lambda 25 spectrometer (Shelton, CT, USA) was used to collect the UV–vis absorption spectra between 200 and 800 nm of graphene materials. 2.3.3. XPS Analysis The analysis of the surface chemistry of GO and GO–AgNPs was performed by XPS on a SPECS system with a monochromatic Al Kα X-ray source (1486.6 eV) and a Phoibos 150 1D-DLD analyzer (Berlin, Germany). The core level spectra were obtained at a photoelectron take-off angle of 90◦, measured with respect to the sample surface. The XPS survey–scan spectra were collected using a pass energy of 80 eV, 1 eV energy step, and 0.1 s dwell time. The individual high-resolution spectra were acquired using a pass energy of 30 eV, 0.1 eV energy step, and 0.1 s dwell time. 2.3.4. Raman Analysis Raman spectra of GO and GO–AgNPs were obtained with a Renishaw Invia microscope (Gloucestershire, UK) with a laser frequency of 514 nm as an excitation source. The spectra were measured from 500 to 3500 cm−1. 2.3.5. XRD Analysis The XRD spectra of graphene materials were recorded using a Malvern Panalytical (Almelo, the Netherlands) X’PERT PRO automatic diffractometer operating at 40 kV and 40 mA in theta–theta configuration, a secondary monochromator with Cu-Kα radiation (λ = 1.5418 Å), and a PIXcel solid state detector (active length in 2θ 3.347◦). Data were collected from 1 to 50◦ 2θ for GO and from 1 to 90◦ 2θ for GO–AgNP samples (step size = 0.026◦ and time per step = 80 s, total time 20 min) at room temperature. A variable divergence slit giving a constant 5 mm area of sample illumination was used. The interlayer separation in the graphene material was calculated by Bragg ́s law (λ = 2d sinθ). 2.3.6. TEM Analysis TEM images were taken using a Philips Tecnai G2 20 TWIN TEM instrument (Eindhoven, the Netherlands) at 200 kV accelerated voltage. A drop of the diluted GO–AgNP nanohybrid suspensions was placed onto coated cooper grids. 2.3.7. Thermogravimetric Analysis (TGA) TGA tests were performed on a TG-Q-500 (TA instruments, New Castle, DE, USA) under nitrogen at a heating rate of 10 ◦C/min, from 40 to 600 ◦C.PDF Image | Graphene Oxide–Silver Nanoparticle Nanohybrids
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