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A Zinc-Rich Coating Fabricated on a Magnesium Alloy by Oxide Reduction

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A Zinc-Rich Coating Fabricated on a Magnesium Alloy by Oxide Reduction coatings Article A Zinc-Rich Coating Fabricated on a Magnesium Alloy by Oxide Reduction Dongzhu Lu 1,2,3,* , Yanliang Huang 1,2,3 , Jizhou Duan 1,2,3 and Baorong Hou 1,2,3 1 CAS Key Laboratory of Marine Environmental Corrosion and Bio-fouling, Institute of Oceanology, Chinese Academy of Science, Qingdao 266071, China; [email protected] (Y.H.); [email protected] (J.D.); [email protected] (B.H.) 2 Open Studio for Marine Corrosion and Protection, Pilot National Laboratory for Marine Science and Technology (Qingdao), Qingdao 266237, China 3 Center for Ocean Mega-Science, Chinese Academy of Sciences, Qingdao 266071, China * Correspondence: [email protected] Received: 1 April 2019; Accepted: 24 April 2019; Published: 25 April 2019 Abstract: The corrosion resistance of magnesium alloys could be enhanced by covering metallic coatings on the surface. The zinc-rich coating is one of these metallic coatings. To fabricate a zinc-rich coating on magnesium alloys, the substrate should be pretreated carefully, and a protective atmosphere is usually required. In this research, a zinc-rich coating was successfully fabricated on the AZ91D magnesium alloy in air by a diffusion alloying method, with zinc oxide as the zinc source. At the same time, the pretreatment of the magnesium alloy matrix was greatly simplified. The as-diffusion-alloyed zinc-rich intermetallic layer was investigated, utilizing SEM, EDS, and XRD, respectively. It is inferred that zinc oxide was reduced into Zn atoms by the active Mg atoms, and the Mg atoms were coming from the magnesium alloy matrix. Then the Zn atoms passed through the oxide film and formed an intermetallic layer on the magnesium alloy surface. Thus, taking advantage of the activity of Mg atoms, magnesium alloys could be surface alloyed with oxides. Keywords: magnesium alloy; zinc oxide; diffusion; coating; surface treatment 1. Introduction Magnesium alloys are lightweight alloys, and could be utilized in various fields [1–3]. The corrosion resistance of magnesium alloys is poor [4–6], which limits further utilization of magnesium alloys. Coatings are fabricated on the surface to enhance the corrosion resistance of magnesium alloys [7–19]. Among which, the zinc coating is an effective one. It is reported that the weight loss of pure Zn is about half of the weight loss of pure Mg in the same duration after exposed to humid air [20]. Adding a little magnesium into pure zinc would reduce the weight loss further [20]. Moreover, zinc-rich coatings are frequently utilized in the electroplating method to fabricate protective coatings on magnesium alloys [17,21]. Magnesium alloys are active, and they are prone to react with oxygen and water to form MgO and Mg(OH)2 on the surface, which would lead to a weak adhesion of as-electrodeposited coatings [17,21]. Thus, before electroplating, magnesium alloys should be pretreated. Zinc immersion is one of the general processes to pretreat magnesium alloys before plating. Before the zinc immersion process, several pretreatment processes, including surface cleaning, alkaline cleaning, acid pickle, and acid activation, are commonly enlisted to remove soil, debris, oil, grease, oxides, etc. [17]. Then the magnesium alloy is immersed in special solutions for the zinc film to form [21]. Coatings 2019, 9, 278; doi:10.3390/coatings9040278 www.mdpi.com/journal/coatings Coatings 2018, 8, x FOR PEER REVIEW 2 of 8 Coatings 2019, 9, 278 2 of 8 grease, oxides, etc. [17]. Then the magnesium alloy is immersed in special solutions for the zinc film to form [21]. The zinc-rich coating could also be fabricated by a thermalthermal evaporationevaporation methodmethod [[18].18]. In this method, a vacuum environment is required, and the temperature for the evaporation of the original Zn powder is 600 °C.◦C. Similarly, the magnesium sp specimenecimen could could be be obtained obtained by by thermal thermal diffusion, diffusion, which buries the magnesium alloy specimen into th thee pure pure Zn Zn powder, powder, and keeps keeps the the diffusion diffusion system system at an elevatedelevated temperaturetemperature for for the the zinc-rich zinc-rich coating coatin tog grow.to grow. In this In this method, meth theod, di theffusion diffusion system system could couldbe buried be buried in compact in compact carbon carbon powder powder to further to further prevent prevent oxidation oxidation [19]. [19]. Thus, it is crucial to clean the surface of a magnesium alloy matrix to prohibit the formation of the magnesium oxide oxide film film in in the zinc immersion method, method, and and it it is is also also crucial crucial to to keep a a relatively inertinert atmosphere, atmosphere, to prohibit the oxidation of pure metals in the the thermal thermal evaporation evaporation method and the the thermal diffusion diffusion method. It It seems seems as as though though oxides oxides are are always always unfavorable, unfavorable, and and should should be be avoided. avoided. In this this research, research, a amethod method based based on onthe thediffusion diffusion alloying alloying process, process, but utilizing but utilizing zinc oxide zinc as oxide the diffusionas the di ffsourceusion sourceinstead insteadof pure ofZn pure powder Zn powderto fabricate to fabricatezinc-rich zinc-richcoatings on coatings magnesium on magnesium alloys, is raised.alloys, isThe raised. pretreatment The pretreatment process of process the magnesium of the magnesium alloy matrix alloy is matrix simplified is simplified effectively eff ectivelyby this method.by this method. Meanwhile, Meanwhile, the environment the environment requirement, requirement, such as a suchvacuum as a or vacuum inert atmosphere, or inert atmosphere, becomes unnecessary.becomes unnecessary. 2. Experimental Experimental Procedures Procedures An as-cast AZ91D magnesium alloy with with the composition of of 9.1 9.1 wt.% wt.% Al, Al, 0.52 0.52 wt.% wt.% Zn, Zn, 0.26 0.26 wt.% wt.% Mn and Mg as balance, balance, was utilized as the matrix. matrix. Samples Samples were were cut cut into into specimens specimens with with a a dimension dimension of 15 mm 10 mm 3 mm from the AZ91D magnesium alloy sheets with an electrical discharge of 15 mm × 10 mm × 3 mm from the AZ91D magnesium alloy sheets with an electrical discharge cutting machine, and and then polished with with SiC papers to 1000 grit, rinsed with alcohol, and naturally dried up. The didiffusionffusion sourcesource isis a a mixture mixture of of 1 1 g g NH NH4Cl4Cl powder powder and and 10 10 g ZnOg ZnO powder. powder. Photographs Photographs of the of theNH NH4Cl4 powderCl powder and and the ZnOthe ZnO powder powder are shownare shown in Figure in Figure1. The 1. magnesium The magnesium alloy specimensalloy specimens were wereinserted inserted in the in di theffusion diffusion source. source. The diTheffusion diffus sourceion source and theandmagnesium the magnesium alloy alloy specimens specimens were were put putinto into a 30 mLa 30 crucible mL crucible for the for following the following heat treatment. heat treatment. A schemetic A schemetic diagram diagram of the di ffofusion the diffusion system is systemshown inis shown Figure2 in. Figure 2. Figure 1. Photographs of the NH 4ClCl powder powder ( (aa)) and and the the ZnO ZnO powder powder ( (bb).). After the furnace temperature reached 430 °C and was kept stable for minutes, the filled crucible was put into the furnace as quickly as possible, and kept at 430 °C for 2 h for the surface alloying process on the magnesium alloy specimen to proceed. The whole surface alloying process was carried out in the air; neither vacuum nor inert gases were utilized. After the surface alloying process, specimens were taken out from the furnace and cooled down naturally in the air. Coatings 2019, 9, 278 3 of 8 Coatings 2018, 8, x FOR PEER REVIEW 3 of 8 Figure 2.2. SchematicSchematic diagram diagram to to show show the the diff usiondiffusion system, system, ZnO wasZnO the was only the Zn only donor Zn in donor the di ffinusion the source,diffusion and source, the di andffusion the alloyingdiffusion process alloying was process carried was out carried directly out in directly the air. in the air. AfterThen the residual furnace temperaturepowder on the reached magnesium 430 ◦C allo andy wasspecimens kept stable was cleaned for minutes, up, and the the filled as-surface crucible wasalloyed put intospecimens the furnace were as washed quickly with as possible, running and wate keptr atand 430 alcohol◦C for 2successively, h for the surface and alloying then naturally process ondried the up. magnesium Cross-sections alloy specimen of the as-surface to proceed. alloyed The wholemagnesium surface alloy alloying specimens process were was carriedobtained out with in the a air;saw. neither Then the vacuum cross-sections nor inert were gases polished were utilized. and et Afterched thesuccessively surface alloying for microstructure process, specimens observation. were takenThe polished out from cross-sections the furnace andwere cooled etched down until naturallythe as-surface in the alloyed air. coating showed up clearly on the specimenThen surface, the residual and then powder washed on the with magnesium alcohol and alloy naturally specimens dried was up. cleaned Microstructure up, and the photographs as-surface alloyedand composition specimens analysis were washed results of with the runningas-diffusion-alloyed water and alcohol specimens successively, were obtained and thenby a naturallyscanning driedelectronic up. microscope Cross-sections (S-3400N, of the as-surfaceHitachi, Tokyo, alloyed Japan). magnesium Phase identification alloy specimens was werecarried obtained out utilizing with aan saw. X-ray Then diffractometer the cross-sections (Ultima were IV, polished Rigaku, and Tokyo, etched Japan). successively The Gibbs for microstructure free energies observation. of relative Thechemical polished reactions cross-sections were calculated were etched by a untilsoftware the as-surface(HSC 6.0).
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