Microstructure, Texture, Mechanical Properties, and Corrosion Behavior of Biodegradable Zn-0.2Mg Alloy Processed by Multi-Directional Forging

doi:10.1007/s40195-024-01792-z

Abstract

Abstract:

This study systematically investigated the microstructure, mechanical properties, and corrosion behavior of an extruded Zn-0.2Mg alloy processed by multi-directional forging (MDF) at 100 °C. The mean grain size was remarkably decreased from 17.2 ± 0.5 µm to 1.9 ± 0.3 µm, and 84.4% of the microstructure was occupied by grains of below 1 µm in size after applying three MDF passes. Electron backscattered diffraction examinations revealed that continuous dynamic recrystallization, progressive lattice rotation, and particle-stimulated nucleation mechanisms were recognized as contributing to microstructural evolution. Furthermore, transmission electron microscopy results showed that nanoparticles of Mg/Zn dynamically formed under high strain MDF, while the initial extrusion fiber texture was altered to be < 0001 > parallel to the final forging axis. A synergistic effect of grain refinement, texture evolution, second-phase precipitates, and dislocation strengthening resulted in an increased ultimate tensile strength of 232 ± 5 MPa after three MDF passes. However, this was accompanied by a reduction in the elongation (8 ± 2.1%). Additionally, a high corrosion rate of 0.59 mm/year was measured for the experimental alloy fabricated by 3 MDF passes. In agreement with the latter, electrochemical impedance spectroscopy results indicated that the grain refinement improved the passivation kinetics of the oxide layer.

Key words: Zinc-based bioalloy, Multi-directional forging (MDF), Microstructure, Recrystallization, Mechanical properties, Corrosion properties

Nafiseh Mollaei, Seyed Mahmood Fatemi, Mohammad Reza Aboutalebi, Seyed Hossein Razavi, Wiktor Bednarczyk. Microstructure, Texture, Mechanical Properties, and Corrosion Behavior of Biodegradable Zn-0.2Mg Alloy Processed by Multi-Directional Forging[J]. Acta Metallurgica Sinica (English Letters), 2025, 38(3): 507-525.

Figures/Tables 20

Fig. 1 Schematic representation of: a MDF corresponding to one pass and b sample extraction for tensile, metallographic, and corrosion testing experiments

Table 1 SBF composition employed in this study

Chemical	MgCl₂∙6H₂O	NaHCO₃	CaCl₂	K₂HPO₄∙3H₂O	NaCl	HCl (1 mol/L)	KCl	Na₂SO₄	TRIS buffer
Amount (/L)	0.311 g	0.352 g	0.293 g	0.23 g	8.036 g	40 ml	0.225 g	0.072 g	6.063 g

Fig. 2 a IPF map, b SEM micrograph, c XRD pattern, d TEM images of the eutectic structure with the corresponding SAED pattern of the network phase, e measured pole figures of the as-extruded Zn-0.2Mg alloy

Fig. 3 Microstructures of the experimental alloy deformed by MDF: a 1 pass; b 2 passes; c 3 passes; d a magnified view of recrystallized grains developed after 3 MDF passes

Fig. 4 TEM micrographs of 3 passes MDFed Zn-0.2Mg alloy: a grains, b dislocations, c dynamic precipitates, d HR-TEM image from the precipitate

Fig. 5 GOS map of the MDFed alloys: a 1 pass, b 2 passes, c 3 passes, d area versus GOS at various deformation passes, e the evolutions of size and fraction of DRX grains as a function of number of passes

Fig. 6 a IPF of the experimental alloy deformed to strain 0.93, b the misorientation profiles along the AB line in a, c the misorientation profiles along the CD line in a

Fig. 7 Inverse pole figure maps representing the PSN mechanism after applying 3 MDF passes on the experimental alloy

Fig. 8 OM and SEM images of the material deformed up: a and b 1 pass, c and d 3 passes

Fig. 9 a EBSD map of deformed grain in the Zn-0.2Mg alloy after two forging passes, b the misorientation gradient measured along A-B line, c the misorientation gradient measured along C-D line, d the crystallographic relationship between P and G. Here, P and G represent parent grains and recrystallized grains, respectively

Fig. 10 Schmid factor distribution of different slip systems in multi-directionally forged Zn-0.2Mg alloy deformed up: a 1 pass, b 3 passes

Fig. 11 {0001} pole figure of the alloy after MDF with different passes: a 1 pass, b 2 passes, c 3 passes

Fig. 12 a Engineering stress vs. engineering strain flow behavior of the as-extruded and MDF-processed materials, b mechanical properties of the studied alloys

Table 2 Average Schmid factors for different slip systems, geometrically necessary dislocation density, and Vickers microhardness of as-extruded and MDF-processed Zn-0.2Mg alloys

Sample	Average SF			Ρ_GND (10¹⁴ m⁻²)	Microhardness (HV)
Sample	Basal	Prismatic	Pyramidal	Ρ_GND (10¹⁴ m⁻²)	Microhardness (HV)
Zn-Mg (AE)	0.39	0.23	0.26	0.03	45 ± 3
Zn-Mg (1 pass)	0.29	0.32	0.39	6.7	54 ± 2
Zn-Mg (2 passes)	0.25	0.38	0.41	5.9	72 ± 3
Zn-Mg (3 passes)	0.23	0.41	0.43	4.1	77 ± 1

Fig. 13 Polarization diagrams of the investigated specimens in SBF solution

Table 3 Electrochemical measurements of the studied specimens in SBF solution

Sample	Corrosion potential E_corr (V vs. SCE)	Current density I_corr (μA/cm²)	Cathodic slope βc (mV)	Anodic slope βa (mV)	Corrosion rate (mm/year)
Pure Zn (AE)	− 0.91 ± 0.17	24.53 ± 2.12	282.75 ± 5.40	52.76 ± 3.51	0.34 ± 0.01
Zn-0.2Mg (AE)	− 1.01 ± 0.01	31.81 ± 4.13	236.32 ± 10.38	209.53 ± 8.60	0.44 ± 0.14
Zn-0.2Mg (1 pass)	− 1.11 ± 0.12	34.63 ± 1.21	392.98 ± 6.50	169.30 ± 6.87	0.48 ± 0.05
Zn-0.2Mg (2 passes)	− 1.17 ± 0.08	37.34 ± 2.35	410.10 ± 12.50	146.98 ± 18.21	0.51 ± 0.08
Zn-0.2Mg (3 passes)	− 1.15 ± 0.03	42.57 ± 3.40	412.92 ± 4.80	193.78 ± 13.36	0.59 ± 0.02

Fig. 14 a SEM images of surface morphologies of the studied specimens after polarization treatment: a pure Zn (AE), b Zn-0.2Mg (AE), c Zn-0.2Mg (1 pass MDF), d Zn-0.2Mg (2 passes), e Zn-0.2Mg (3 passes)

Table 4 Results of EDS analysis of corrosion products formed on the investigated samples (wt%)

Samples	Zn	O	Cl	P	Ca	Mg
Pure Zn (AE)	61.49	28.89	2.99	1.66	4.26	0.71
Zn-0.2Mg (AE)	61.68	36.35	0.55	1.30	0	0.11
Zn-0.2Mg (3 passes MDF)	60.16	41.74	0.19	1.019	0.72	0.08

Fig. 15 EIS diagrams in SBF solution at 37 °C for Pure Zn, Zn-0.2Mg, and 3 passes MDFed Zn-0.2Mg: a Nyquist plots, b Bode magnitude plots, c Bode phase plots, d equivalent circuit

Table 5 EIS parameters obtained in SBF solution at 37 °C from equivalent circuits of Rs(Qct(Rct ZW)) for pure Zn, Zn-0.2Mg, and Zn-0.2Mg (3 passes) alloys

Specimens	R_s (Ω cm²)	R_ct (kΩ cm²)	Q_ct		Z_W
Specimens	R_s (Ω cm²)	R_ct (kΩ cm²)	Y₀ (Ω⁻¹ cm⁻² s⁻ⁿ)	n	Z_W
Pure Zn (AE)	107 ± 2	9.95 ± 0.12	0.73 ± 0.01	0.71 ± 0. 04	0.00032
Zn-0.2Mg (AE)	112 ± 1	7.53 ± 0.24	0.64 ± 0.03	0.78 ± 0.03	0.00045
Zn-0.2Mg (3 passes)	108 ± 1	4.21 ± 0.31	0.49 ± 0.01	0.83 ± 0.01	0.00061

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