Paper_Fast and inexpensive synthesis of multilayer graphene used as Pd support in alkaline direct ethanol fuel cell anode
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Dados originais referentes a medidas e resultados obtidos para a produção do artigo científico "Síntese rápida e econômica de grafeno multicamadas usado como suporte de Pd em ânodo de célula a combustível de etanol direto alcalino".
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Fast and inexpensive synthesis of multilayer graphene used as Pd support in alkaline direct ethanol fuel cell anode Experimental characterization 2.3.1. X-ray diffraction (XRD) All electrocatalysts were physically characterized using X-ray diffraction (XRD). A Rigaku-MiniFlex X-ray diffractometer with a CuKα (λ = 1.54056 Å) radiation source using an increment of 2° min-1 from 20º to 80° (2θ). 2.3.2. Elemental composition by ICP-MS analysis The elemental composition of the electrocatalyst was determined using an inductively coupled plasma mass spectrometer (ICP-MS, Agilent 7900, Hachioji, Japan) with high-purity argon (99.9999%, White Martins, Brazil). All reagents were of analytical grade. Nitric acid and HCl were purified by using a Teflon sub-boiling distiller (DST-100, Savillex, USA). High-purity deionized water (resistivity 18.2 MΩ cm) was generated with a Milli-Q water purification system (Millipore, Bedford, MA, USA). The Pd extraction was carried out using a closed vessel system. Approximately 30 mg of electrocatalyst was placed into 100 mL tubes that contained 3 mL of HNO3 + 1 mL of HCl, and the tubes were then closed. Then, the tubes stood for 24 h at 25 °C. After this step, they were heated at 200 °C for 2 h in a graphite-covered digester block (EasyDigest, Analab, France). Finally, the volume was increased to 50 mL, and the elemental composition was determined by ICP-MS. The calibration curve ranged from 1-50 µg L-1 for Pd and Nb and resulted in R2 = 0.9999. All the conditions for these measurements were described earlier in our previous publications [13, 39]. 2.3.3. Transmission electron microscopy (TEM) To determine the particle size and morphology, the transmission electron microscopy (TEM) analysis was carried out using a high-resolution TEM (JEOL model JEM 2100F) operating at 200 kV. Samples for TEM studies were prepared as before [13]. The compositional distribution (mapping) and the average particle size was performed like references [13]. 2.3.4. Contact Angle The hydrophilicity of materials and electrocatalysts were performed using a goniometer (GBXTM digidrop) as reported in previous work [13]. 2.3.5. Raman Spectroscopy The Raman spectra were recorded using a Triple T64000 Raman spectrometer (Horiba Jobin-Yvon S.A.S., France) with a microanalysis option and a CCD detector (1024×256—OPEN-3LD/R) with a quantum response of ∼40% and a spectral resolution of 0.5 cm-1. The excitation laser was 532 nm (Verdi G5, Coherent Inc., United States) was focused on a spot size of 50 mm. The experiments were performed according to our previous publication [38].