The Effect of Pore Sealing in a Multilayer Si–O–Zr/Al2O3 Coating Designed to Protect Aluminium from Corrosion

• Published in: Metals (Basel ) Vol. 13; no. 12; p. 1960
• Main Authors: Rodič, Peter, Kapun, Barbara, Milošev, Ingrid
• Format: Journal Article
• Language: English
• Published: Basel MDPI AG 01.12.2023
• Subjects: aluminium; Aluminum oxide; atomic layer deposition; Atomic layer epitaxy; corrosion; Corrosion potential; Corrosion prevention; Corrosion tests; Electrochemical impedance spectroscopy; hybrid sol–gel; Infrared spectroscopy; Ion beams; Metals; Methacrylic acid; Multilayers; pore sealing; Protective coatings; Sealing; Sodium chloride; Sol-gel processes; Sols; Spectrum analysis; Substrates; Temperature; Tetraethyl orthosilicate; Thin films; X-ray spectroscopy; Zirconium; United States > US
• ISSN: 2075-4701; 2075-4701
• DOI: 10.3390/met13121960

This study deals with the combination of two corrosion protection strategies for aluminium: barrier protection (provided by a 3.8 μm thick hybrid sol–gel coating) and aluminium pore sealing via the use of a 100 nm thick layer of aluminium oxide. A Si–O–Zr hybrid sol–gel coating (TMZ) was synthesised by combining two separately prepared sols (i) tetraethyl orthosilicate and 3-methacryloxypropyl trimethoxysilane and (ii) zirconium(IV) n-propoxide chelated with methacrylic acid. The synthesis of the Si–O–Zr hybrid sol–gel was evaluated at various stages using real-time infrared spectroscopy. A 100 nm thick Al2O3 film was prepared via thermal atomic layer deposition at 160 °C using trimethyl aluminium and water as precursors. The coating and film properties were assessed via focused ion beam/scanning electron microscopy coupled with energy-dispersive X-ray spectrometry. Sealing with the Al2O3 film did not affect the microstructure and composition of the underlying sol–gel coating. The coating’s corrosion performance in 0.1 M NaCl solution was evaluated using electrochemical impedance spectroscopy. Compared to individual coatings, the multilayer TMZ/Al2O3 coating ensured prolonged (more than three weeks) durable corrosion protection for the aluminium. The impedance magnitude increased by two orders compared to the uncoated substrate (|Z|10 mHz from 16 kΩ cm2 to almost 830 MΩ cm2). Thus, the pore sealing of the sol–gel coating using an ALD alumina film produced a protective multilayer coating system, with |Z|10 mHz remaining above 5 MΩ cm2 after four weeks in NaCl solution.