Surfactant Modified Alumina Lab Report

Preparation of template
The surfactant modified alumina template was prepared by precipitation method previously reported in literature []. Typically, Precursor solution and surfactant solution were prepared by dissolving required amount of aluminium nitrate nonahydrate and sodium dodecyl sulfate in distilled water. Molar composition ratio of both the aluminium precursor and surfactant solutions was taken as 4:1. Mixture was stirred for 15 minutes at room temperature then precipitation was carried out by gradual addition of 30% ammonia solution at pH of 10.5. The subsequent steps of aging, filtering, washing and drying were same as followed. The calcination was carried out at 550 °C for 4 h. The prepared SDS surfactant modified alumina referred
The required amount of Pt, Pd and Ni nitrates precursor were immersed in deionised water. The precursor solution was dispersed drop wise to template. Finally, the obtained metals-doped templates were heated at 120 oC for 12 h. The resulting metals containing alumina-SDS templates was placed in horizontal furnace for the synthesis of metal and nitrogen doped templated carbons and followed same procedure as described in section 2.2 above. The metals (Pt, Pd & Ni) content was maintained at 1.5wt %. The 0.5 and 1wt % of Pd content was doped on template. The final doping and presence of metals was confirmed by EDX and XRD analysis.
The samples synthesized were denoted as AlS-N, Pt/AlS-N, Ni/AlS-N and Pd/AlS-N. AlS represented as alumina with SDS and N stand for doped nitrogen. Whereas, Pt, Ni and Pd indicated as doped platinum, nickel and palladium. The carbon yields for different synthesis templated carbons were calculated based on amount of template used and defined as
Y
Thermogravimetric analysis (TGA) of template for thermal stability was performed using TG, Netzsch instrument with heating rate of 10oC/min under nitrogen flow with temperature range of 30 to 900 oC. The textural properties were determined using nitrogen adsorption/desorption isotherms measured with a Quantachrome Autosorb iQ instrument at 77 K. Before each analysis, the samples were evacuated for 3 h at 200 oC under helium atmosphere. The BET surface area was calculated by the Brunauer-Emmett-Teller (BET) method based on adsorption data in the relative pressure (Ps/Po) range 0.05-0.30. The total pore volume was determined from the amount of nitrogen gas adsorbed at (Ps/Po) 0.99. Micropore surface area was obtained via t-plot analysis. The pore size distributions were determined by density functional theory (DFT) model using nitrogen adsorption data. High resolution X-ray powder diffraction spectra were recorded using a Bucker D8 advance diffractometer with Cu–Kɑ radiation operating at 40 kV and 40 mA. The average crystallite size of samples was calculated using Scherer’s formula. Raman spectra of templated carbons were taken in a Jobin-Yvon T6400 laser micro-Raman system. We used a green with wavelength of 514 nm line of Ar-Cd laser as the excitation source. Before Raman analysis, the samples were manually