Synthesis of super-hydrophobic carbonaceous materials is gaining a broader interest by the research community due to its versatile application in separation processes, special coating technologies, and membrane distillation. Carbon nanomaterials (CNMs) may exhibit stable super-hydrophobic character due to their unique physio-chemical features which can be further controlled based on customer requirements by optimizing the process variables. This study deals with the application of a bimetallic catalyst composed of iron (Fe) and cobalt (Co) to synthesize CNMs from powder activated carbon as a precursor. The process parameters were optimized to ensure super-hydrophobic surfaces. Chemical vapor deposition was utilized for the growth of carbon nanomaterials. The impact of input variables on the desired output of yield and contact angle was analyzed. The chemical vapor deposition process was optimized using the response surface methodology based on Box-Behnken design. The proportion of the catalysts and reaction time were the three input explanatory variables whereas the desired response variables were selected as the carbon yield (CY) and contact angle (CA). The synthesized super-hydrophobic materials were characterized using field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), Raman spectroscopy, thermogravimetric analysis (TGA), and contact angle analysis. The comprehensive statistical study of the results led to a significant model and optimization. The highest CY (351%) and CA (173◦ ) were obtained at the optimal loading of 2.5% Fe and 2% Mo with a reaction time of 60 min. The images obtained from FESEM and TEM revealed the presence of two types of CNMs including carbon nanofibers and multiwall carbon nanotubes. Thermogravimetric analysis was carried out to observe the temperature degradation profile of the synthesized sample. Raman spectroscopic analysis was also used to observe the proportion of ordered and disordered carbon content inside the synthesized samples. The improved catalytic super-hydrophobic carbon nanostructured materials production process proposed by this study assures the stability and high yield of the product.
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