Abstract
The impact of multi-directional compression passes on the microstructure, mechanical properties, and corrosion behavior of ZK60 magnesium alloy was investigated. Results reveal that severe dendrite segregation exists in the as-cast ZK60 magnesium alloy with coarse MgZn phases distributed along the grain boundaries. After 9 passes of compression, the coarse solidified phases at the grain boundary are significantly refined, and back dissolution occurs. Fine recrystallized grains accompanied with the fine diffused nano-phases emerge in the local area around the large grains. The tensile strength of ZK60 magnesium alloy generally exhibits the upward trend with the increase in compression passes, whereas the compression rate shows the downward trend. The compressive strength reaches 433.6 MPa with the compression rate of 21.3% after 9 passes of compression. Multi-directional compression can significantly reduce the degradation rate of ZK60 magnesium alloy in simulated body fluids. Furthermore, it is observed that in the as-cast ZK60 magnesium alloy, micro-segregation can easily lead to severe intragranular local corrosion. However, after multi-directional compression, the tendency to intragranular local corrosion is significantly diminished.
Magnesium alloys, as implant materials, exhibit excellent biocompatibility and can be degraded in the human body, becoming the frontier in biomedical materials. Nevertheless, magnesium alloy have encountered notable challenges when used for internal fracture of fixation
Research findings indicate that both the strength and toughness of magnesium alloys can be significantly enhanced by deformation process. Furthermore, the meticulously tailored deformation process has been proven to improve the corrosion resistance of magnesium alloy
Multi-directional compression technique, as conventional plastic deformation process, offers the advantages of easy operation, simple processing and high cost-effectiveness. Utilizing existing industrial equipment, this technique can prepare plastic deformation materials with large volume and excellent performance, thereby directly achieving large-scale industrial productio
When alloys are directly subjected to multi-directional compression without pre-solidification or softening treatments, the synergistic effect of force and heat leads to fracture and re-dissolution of the second phases, thus making early heat treatment unnecessary. This not only enhances processing efficiency but also avoids excessive grain growth caused by early heat treatment. ZK60 magnesium alloy, distinguished by excellent mechanical properties and high specific strength, is extensively used in various applications. However, research on the influence of direct multi-directional compression on the mechanical properties and corrosion resistance of ZK60 magnesium alloy is rare. Consequently, this study focused on the as-cast ZK60 magnesium alloy, which is primarily composed of Mg, Zn, and Zr, and investigated the microstructural changes and their influence on mechanical properties and corrosion resistance under varying compression passes through direct multi-directional compression. The ultimate goal is to design the processing technique for deformed ZK60 magnesium alloy, characterized by superior mechanical properties and corrosion resistance. Such insights provide significant reference for the design of multi-directional compression processes and improvement of corrosion resistance of Mg-Zn-Zr series magnesium alloys.
Commercial as-cast ZK60 magnesium alloy with a chemical composition of Mg-5.20Zn-0.45Zr-0.01Fe-0.01Ni-0.01Cu (wt%) was selected as the raw material for the com-pression experiment. The as-cast ZK60 magnesium alloy used for the multi-directional compression experiment had dimen-sions of 20 mm×20 mm×17 mm, as shown in

Fig.1 Schematic diagram of compression sample

Fig.2 Schematic diagram of the thermal compression device
Upon reaching the required temperature of experiment, the furnace was opened to place the samples. After the samples were kept at the experiment temperature for 5 min, the compression experiment started. After one compression test, the sample was quenched in water. Following the compression experiment in the specific axial direction of the sample, the compression axis was rotated by 90° and the procedure was repeated for the next compression test. In this study, the compression ratio was calculated as 20% of the axial length for each compression.
After the multi-directional compression experiment, the sample was cut into two parts (

Fig.3 Schematic diagram of sampling
X-ray diffraction (XRD, DX-2700B) with Cu-Kα radiation was used to characterize the phase composition of the samples before and after compression. The scanning range of the diffraction angle 2θ was 20°–100°, the scanning speed was 4°/min, and the working voltage was 30 kV. The microstructure and composition of the samples were observed by scanning electron microscope (SEM, Hitachi SU5000) and transmission electron microscope (TEM, FEI Talos F200X). The samples were mechanically thinned to thickness of 200 μm and then ion thinning was performed. The dislocation, grain, grain boundary, and second phase particles of the samples were mainly observed.
The room temperature compression test of the sample was conducted in accordance with the relevant standard of GB/T7314-2005 “Metallic materials-Compression test method at room temperature”. The sample was the cylinder with diameter of 4 mm and height of 5 mm. The room temperature compression test was conducted with the test machine WDW-100A, and the compression rate was 3×1
The electrochemical test of samples was conducted on CS-350PA-type electrochemical workstation. Before the test, the surface of the sample was finely ground with 600#, 1000#, and 1200# metallographic sandpaper, followed by cleaning with deionized water and alcohol, and drying with hairdryer in cold air. The standard three-electrode system was adopted in the electrochemical experiment. The sample to be tested was the working electrode, the platinum electrode was the auxiliary electrode, and the reference electrode was saturated calomel, which was tested in Hank's solution (8.0 g/L NaCl, 0.4 g/L KCl, 0.06 g/L Na2HPO4, 0.06 g/L KH2PO4, 0.35 g/L NaHCO3, 0.2 g/L MgSO4·7H2O, 0.14 g/L CaCl2). Firstly, the sample was immersed in Hank's solution for the open-circuit potential (OCP) test. After OCP value of the sample was stabilized, the electrochemical impedance spectroscopy (EIS) test was conducted. The scanning frequency of the test was 1
The solution used for immersion experiment contained the same composition as that used for the electrochemical experiment, which was Hank's solution. To create the immersion environment that closely matched the real human body environment, the thermostatic water bath was used to maintain the temperature of the immersion solution at 37 °C. The solution was replaced every 24 h during the experiment. The ratio of the exposed surface area of the test sample to the volume of simulated body fluid was 1 c
The sample used for the immersion experiment was a cube of 3 mm×7 mm×9 mm, and the six surfaces of the cube were finely ground with 2000# metallography sandpaper. After immersion, the sample was ultrasonically cleaned for 10 min with the mixture of 200 g·
The corrosion rate of the alloy is calculated, as follows:
(1) |
where CR is the average mass loss corrosion rate (mm/a), ΔW is the mass difference of the sample before and after immersion test (g), A is the surface area of the sample exposed to the solution (c

Fig.4 OM images of ZK60 magnesium alloy at different states: (a) as-cast; (b) 3 passes; (c) 6 passes; (d) 9 passes

Fig.5 Average grain sizes of ZK60 magnesium alloys at different states
The phenomenon of dynamic recrystallization in metal can only occur when the critical deformation amount is reached, and the deformation temperature is higher. At the compression temperature of 350 °C, the substantial deformation of ZK60 magnesium alloy is achieved with the increase in deformation passes. Numerous deformation defects such as dislocations and subgrain boundaries are introduced into the deformed magnesium alloy matrix, which can be eliminated through the nucleation and grain growth of dynamic recrystallization. The primary mechanism can be explained as follows. After large plastic deformation, numerous high-density dislocation regions are formed in the alloy, leading to local migration of grain boundaries and the formation of bump

Fig.6 SEM images of ZK60 magnesium alloy at different states: (a) as-cast; (b) 3 passes; (c) 9 passes
After 3 passes of multi-directional compressions (
XRD patterns of as-cast ZK60 magnesium alloy before and after multidirectional compression are shown in

Fig.7 XRD patterns of ZK60 magnesium alloy at different states

Fig.8 TEM images of ZK60 alloy after 9 passes of multi-directional compression: (a) dislocation; (b–c) dynamic recrystallization grains and dispersion of precipitates
In
Spot | Mg | Zn |
---|---|---|
1 | 50.37 | 49.62 |
2 | 94.71 | 5.29 |

Fig.9 TEM image (a) and EDS element mappings (b‒d) of ZK60 alloy after 9 passes of multi-directional compression: (b) Mg, (c) Zn, and (d) Zr

Fig.10 Engineering stress-engineering strain curves of ZK60 magnesium alloys at different states
State | Yield strength/MPa | Compressive strength/MPa | Elongation/% |
---|---|---|---|
As-cast | 131.5±1.1 | 372.9±2.1 | 23.5±2.3 |
3 passes | 134.7±2.3 | 399.1±1.6 | 27.6±1.7 |
6 passes | 173.5±2.9 | 387.0±2.6 | 25.1±1.6 |
9 passes | 199.1±2.1 | 433.7±1.6 | 20.6±2.1 |
The accumulation of substantial strain during multi-pass and multi-directional deformation refines the microstructure of the alloy. External compression results in refined grains, signifying the presence of more grain boundaries that impede
crack expansion. Moreover, multi-directional compression and the fine dispersed solidification precipitates contribute to the dispersion strengthening effect. Notably, the grain boundary and the precipitated fine dispersed nano-phase (
The polarization curves of as-cast ZK60 magnesium alloy before and after different passes of multi-directional com-pression are depicted in

Fig.11 Polarization curves of ZK60 magnesium alloys at different states
State | Self-corrosion potential, Ecorr/V vs. SCE | Self-corrosion current density, icorr/μA·c |
---|---|---|
As-cast | -1.3924 | 53.59 |
3 passes | -1.3317 | 25.40 |
6 passes | -1.3532 | 36.78 |
9 passes | -1.3869 | 38.34 |
These findings highlight the influence of multi-pass compression deformation on the corrosion behavior of ZK60 magnesium alloy. The increasing absolute value of self-corrosion potential and the decreasing self-corrosion current density suggest that corrosion resistance is improved with the increase in compression passes, providing valuable insights for the development of corrosion-resistant magnesium alloys for various applications.

Fig.12 Corrosion rates of ZK60 magnesium alloys at different states
These results underscore the impact of multi-directional compression deformation on the corrosion behavior of ZK60 magnesium alloy in simulated body fluid. The marginal decrease in corrosion rate of the alloy after 6 com- pression passes indicates that corrosion resistance is enhanced, providing valuable insights for the development of corrosion-resistant magnesium alloys for biomedical applications.
The morphologies of the as-cast ZK60 magnesium alloy after corrosion in simulated body fluid are shown in

Fig.13 Corrosion morphologies of as-cast ZK60 magnesium alloys after removing corrosion products
Point | Mg | Zn | Zr |
---|---|---|---|
1 | 94.47 | 5.53 | 0.00 |
2 | 95.01 | 3.61 | 1.38 |

Fig.14 Schematic diagrams of corrosion process of as-cast ZK60 magnesium alloy

Fig.15 Corrosion morphologies of as-cast ZK60 magnesium alloys at different states after removing corrosion products: (a–b) 3 passes; (c–d) 6 passes; (e–f) 9 passes
After 6 and 9 passes of multi-directional compressions, the morphologies of ZK60 magnesium alloy are depicted in
In conclusion, it is evident that for the ZK60 magnesium alloy, the corrosion resistance exhibits the trend of initial enhancement followed by decrease with the increase in multi-directional compression passes, although it generally surpasses that of the as-cast alloy. This phenomenon is attributed to the presence of dendrite segregation in the ZK60 magnesium alloy and the enrichment of Zn element at the edges of the dendrite arms. Furthermore, solidification precipitates with various sizes and shapes are present in the grain boundaries and intracrystalline dendrites, and the electrode potential in these regions is higher than that of the dendrite arms, leading to micro-galvanic corrosion. Initially, dendrite corrosion occurs, as shown in
After 3 passes of multi-directional compression, the structure of as-cast alloy undergoes significant changes due to the combined influence of heat and forces of multi-directional compression. Initially, the solidified precipitates break and redissolve. Concurrently, Zn atoms diffuse from high to low concentration zones, leading to the substantial reduction in dendrite segregatio
1) The dendrite segregation of ZK60 alloy is reduced after multi-pass and multi-directional compression. After 9 passes of multi-directional compression, recrystallized grains appear around the large grains, and there are fine dispersed nano-phase precipitation around the grains.
2) The compressive strength of ZK60 magnesium alloy exhibits substantial increase with the increase in com- pression passes. With 9 passes of compression, the yield strength of ZK60 alloy rises from 131.5 MPa to 199.1 MPa, and the compressive strength increases from 372.9 MPa
to 433.7 MPa.
3) After multi-directional compression, the local corrosion tendency of ZK60 alloy is reduced, and the average corrosion rate of ZK60 alloy is the lowest of 0.424 mm/a after 3 passes of compression.
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