The present study reports the effect of phosphorus content in deposited electroless nickel (Ni–P) coatings, the heat treatment on the microhardness and its microstructural characteristics, and the influence of the temperature on the microstructure of the Mg alloy substrate during the heat treatment. The deposition of Ni–P coatings was carried out in the electroless nickel bath, and the resulting P content ranged from 5.2 to 10.8 wt.%. Prepared samples were heat-treated in the muffle furnace at 400 °C for 1 h after the coating deposition. The cooling of the samples to room temperature was proceeded in the air. For as-deposited and heat-treated samples, it was determined that with the increasing P content, the microhardness was decreasing. This may be caused by the changes in the structure of the Ni–P coating. The X-ray diffraction patterns of the as-deposited Ni–P coatings showed that the microstructure changed their nature from crystalline to amorphous with the increasing P content. The heat treatment of prepared samples led to the significant increase of microhardness of Ni–P coatings. All the heat-treated samples showed the crystalline character, regardless of the P content and the presence of hard Ni3P phase, which can have a positive effect on the increase of microhardness. The metallographic analysis showed changes of substrate microstructure after the heat treatment. The prepared coatings were uniform and with no visible defects.
Magnesium with its mechanical properties and nontoxicity is predetermined as a material for biomedical applications; however, its high reactivity is a limiting factor for its usage. Powder metallurgy is one of the promising methods for the enhancement of material mechanical properties and, due to the introduced plastic deformation, can also have a positive influence on corrosion resistance. Pure magnesium samples were prepared via powder metallurgy. Compacting pressures from 100 MPa to 500 MPa were used for samples’ preparation at room temperature and elevated temperatures. The microstructure of the obtained compacts was analyzed in terms of microscopy. The three-point bendisng test and microhardness testing were adopted to define the compacts’ mechanical properties, discussing the results with respect to fractographic analysis. Electrochemical corrosion properties analyzed with electrochemical impedance spectroscopy carried out in HBSS (Hank’s Balanced Salt Solution) and enriched HBSS were correlated with the metallographic analysis of the corrosion process. Cold compacted materials were very brittle with low strength (up to 50 MPa) and microhardness (up to 50 HV (load: 0.025 kg)) and degraded rapidly in both solutions. Hot pressed materials yielded much higher strength (up to 250 MPa) and microhardness (up to 65 HV (load: 0.025 kg)), and the electrochemical characteristics were significantly better when compared to the cold compacted samples. Temperatures of 300 °C and 400 °C and high compacting pressures from 300 MPa to 500 MPa had a positive influence on material bonding, mechanical and electrochemical properties. A compacting temperature of 500 °C had a detrimental effect on material compaction when using pressure above 200 MPa.
The use of zinc-based materials as biodegradable materials for medical purposes is offered as a possible alternative to corrosion-less resistant magnesium-based materials. Zinc powders with two different particle sizes (7.5 µm and 150 µm) were processed by the methods of powder metallurgy: cold pressing, cold pressing followed by sintering and hot pressing. The microstructure of prepared materials was evaluated in terms of light optical microscopy, and the mechanical properties were analyzed with Vickers microhardness testing and three-point bend testing. Fractographic analysis of broken samples was performed with scanning electron microscopy. Particle size was shown to have a significant effect on compacts mechanical properties. The deformability of 7.5 µm particle size powder was improved by increased temperature during the processing, while in the case of larger powder, no significant influence of temperature was observed. Bending properties of prepared materials were positively influenced by elevated temperature during processing and correspond to the increasing compacting pressures. Better properties were achieved for pure zinc prepared from 150 µm particle size powder compared to materials prepared from 7.5 µm particle size powder.
Superhydrophobic surfaces were prepared using a two-step method that involved the etching of AZ31 and AZ91 magnesium alloys and then modifying the etched alloys with stearic acid. Magnesium alloys etched with ZnCl2 and SnCl2 exhibited surfaces roughened with micro- and nanoscale hierarchical structures consisting of two chemically distinct regions (Zn/Zn(OH)2 or Sn/SnO2 and Mg(OH)2). An optimum etching time of ten minutes was chosen for both etchants. Superhydrophobic surfaces with the highest contact angle were prepared when stearic acid reacted with the etched alloys at 50 °C for 4 h. Stearic acid was bound as zinc stearate and magnesium stearate on Mg alloys etched with ZnCl2 and SnCl2 solutions, respectively. The superhydrophobic process on AZ31 alloys etched with ZnCl2 and SnCl2 improved the corrosion resistance in phosphate buffered saline (PBS) solution compared to bare AZ31 alloy, with the use of ZnCl2 etchant leading to better results. An improvement in the corrosion resistance of AZ91 alloy was observed when the stearic-acid-modified AZ91 alloy was etched with SnCl2. In contrast, the use of ZnCl2 etchant to pretreat AZ91 alloy resulted in a significant deterioration in corrosion properties compared to bare AZ91 alloy. The microstructure of the Mg alloy had an impact on the etching and modification process. On the basis of the findings, a characterization of the chemistry of etching magnesium alloys and the formation of superhydrophobic surfaces was proposed. Magnesium alloys were prepared with superhydrophobic surfaces, incorporating antibacterial metals, features which may increase their potential for use in medical applications.
The main advantage of magnesium and its alloys is high specific strength and biocompatibility. A modern approach to magnesium-based materials preparation is powder metallurgy. This technique allows preparation of new materials with a unique structure, chemical composition, and controlled porosity. In this study, cold compaction of magnesium powder was studied. Magnesium powder of average particle size of 30 μm was compacted applying pressures of 100 MPa, 200 MPa, 300 MPa, 400 MPa and 500 MPa at laboratory temperature. Influence of compacting pressure was studied with microstructural and electrochemical corrosion characteristics analysis. The resulting microstructure was studied in terms of light and electron microscopy. Obtained electrochemical characteristics were compared with those of wrought magnesium. Compacting pressure had a significant influence on microstructure and electrochemical characteristics of prepared bulk magnesium. With the increase in compaction pressure, the porosity decreased. Compacting pressures of 300 MPa, 400 MPa and 500 MPa led to the similar microstructure of the prepared material. Polarization resistance of compacted magnesium was much lower and samples degraded faster when compared to wrought magnesium. Also, the corrosion degradation mechanism changed due to the microstructural differences between the material states.
Pure Mg samples were prepared by powder metallurgy using the cold and hot compacting methods. Cold compacted pure Mg (500 MPa/RT) was characterized by 5% porosity and the mechanical bonding of powder particles. Hot compacted samples (100 MPa/400 °C and 500 MPa/400 °C) exhibited porosity below 0.5%, and diffusion bonding combined with mechanical bonding played a role in material compaction. The prepared pure Mg samples and wrought pure Mg were subjected to corrosion tests using electrochemical impedance spectroscopy. Similar material corrosion behavior was observed for the samples compacted at 500 MPa/RT and 100 MPa/400 °C; however, hot compacted samples processed at 500 MPa/400 °C exhibited longer corrosion resistance in 0.9% NaCl solution. The difference in corrosion behavior was mainly related to the different binding mechanisms of the powder particles. Cold compacted samples were characterized by a more pronounced corrosion attack and the creation of a porous layer of corrosion products. Hot compacted samples prepared at 500 MPa/400 °C were characterized by uniform corrosion and the absence of a layer of corrosion products on the specimen surface. Powder-based cold compacted samples exhibited lower corrosion resistance compared to the wrought pure Mg, while the corrosion behavior of the hot compacted samples prepared at 500 MPa/400 °C was similar to that of wrought material.