Preparation of Al2O3 coating on TiN coating by polymer-assisted deposition to improve oxidation resistance in coking inhibition applications

Abstract

In order to inhibit the metal catalytic coking and improve oxidation resistance of single TiN coating, the TiN/Al2O3 double layer coatings were designed as a chemically inert coating for methylcyclohexane supercritical pyrolysis. Internal TiN coatings were prepared by atmospheric pressure chemical vapor deposition using TiCl4–H2–N2 system. The external Al2O3 coatings with different thicknesses were prepared on the TiN surface by polymer-assisted deposition, and the coating with the most suitable thickness was further annealed at different temperatures of 600, 700, 800 and 900 °C. The morphology, elemental and phase composition of TiN/Al2O3 coatings were characterized by SEM, EDX and XRD respectively. The chemical state information of the coating elements was based on Ti 2p, Al 2p core level X-ray photoelectron spectroscopy (XPS) spectra. The results indicated that the external Al2O3 coating will partially peel off at 900 °C annealing temperature. The thermogravimetric analysis results indicated that all TiN/Al2O3 coatings show better oxidation resistance than single-layer TiN coating. The anti-coking test with methylcyclohexane supercritical pyrolysis showed that the TiN/Al2O3 coatings can effectively cover the metal catalytic sites and eliminate metal catalytic coking. However, the acid sites of external Al2O3 coating slightly promoted coking, so the anti-coking ratios of TiN/Al2O3 coatings were smaller than that of TiN. Thus, the addition of external Al2O3 coating can greatly improve the oxidation resistance of TiN coatings with little loss of coking resistance.