Effect of Sintering Time on the Mechanical and Corrosion Behavior of Zn-Mg Composites with a Core-Shell Structure Prepared by SPS

doi:10.1007/s40195-023-01548-1

Abstract

Abstract:

Zn-10 Mg composite with a core-shell structure was prepared by spark plasma sintering (SPS) technology, and a systematic study of the microstructure and properties has been conducted for different sintering times. The shell layer dominated by the hard MgZn₂ phase thickens with the increase in sintering time, which has a positive effect on the mechanical and degradation properties of the material. The sample sintered for 20 min (T-20) has the best mechanical properties, with a compressive strength of 226 MPa and a compression rate of 6.5%. The corrosion resistance of samples increases as the sintering time prolongs, while the hydrogen evolution volume and pH value decrease in the immersion experiment. Furthermore, the increase in the shell thickness significantly reduces the corrosion rate, which is attributed to the weakening of the galvanic corrosion reaction between the Mg core and the MgZn₂ shell. Therefore, composite with unique core-shell structure provides an advanced design idea for degradable biomaterials, and a reasonable control of sintering time can provide the optimal design strategy.

Key words: Zn-Mg composite, Spark plasma sintering (SPS), Core-shell structure, Mechanical property, Degradation mechanism

Zeqin Cui, Lei Zhou, Xiaohu Hao, Mengda Luo, Wenxian Wang, Jianzhong Wang, Weiguo Li. Effect of Sintering Time on the Mechanical and Corrosion Behavior of Zn-Mg Composites with a Core-Shell Structure Prepared by SPS[J]. Acta Metallurgica Sinica (English Letters), 2023, 36(8): 1305-1316.

Figures/Tables 13

Fig. 1 Raw material powders: a SEM image of Zn powders, b distribution of Zn powders size, c SEM image of Mg powders, d distribution of Mg powders size

Fig. 2 Temperature-pressure-time curves for SPS

Fig. 3 Microstructures of the Zn-10 Mg composite: a OM image, b quantitatively analysis points A, B, and C in the image of the core-shell interface in the upper right corner, c scanning results of region A of TEM slices at the core-shell interface, d local magnification of region B (shell) in (c), e selected electron diffraction patterns in the region B (shell), f XRD image

Fig. 4 SEM images of Zn-10 Mg composites prepared at different sintering times

Table 1 Relative density of materials after sintering

Material	Density (g/cm³)	Relative density (%)
T-10	5.38	98.7 ± 0.003
T-15	5.39	98.9 ± 0.025
T-20	5.41	99.3 ± 0.033
T-25	5.42	99.4 ± 0.062

Fig. 5 Mechanical properties of composites made at different sintering times: a Vickers hardness, b compressive stress-strain curves, c flexural strength and flexural modulus, *p < 0.05, compared with T-10

Table 2 Compression properties of samples prepared at different sintering times

Materials	Compressive strength (MPa)	Yield strength (MPa)	Compression rate (%)
T-10	216 ± 2.14	200 ± 0.34	5.9 ± 0.070
T-15	219 ± 1.50	210 ± 0.13	6.2 ± 0.048
T-20	226 ± 1.22	217 ± 0.99	6.5 ± 0.069
T-25	208 ± 2.90	200 ± 0.98	5.8 ± 0.109
Cortical bone	130-180 [24]	164-240 [25]	1.81-1.89

Fig. 6 Fracture morphologies of samples prepared at different sintering times: a 10 min, b 15 min, c 20 min, d 25 min

Fig. 7 Corrosion behaviors of studied materials based on electrochemical tests: a potentiodynamic polarization curves, b Nyquist plots

Table 3 Electrochemical corrosion parameters of samples in SBF

Materials	E_corr (V)	I_corr (μA cm⁻²)	R_p (kΩ cm⁻²)
T-10	− 1.198 ± 0.011	126.207 ± 1.345	5.425 ± 0.026
T-15	− 1.183 ± 0.028	123.756 ± 2.167	5.548 ± 0.054
T-20	− 1.180 ± 0.002	124.106 ± 0.894	5.553 ± 0.015
T-25	− 1.170 ± 0.009	121.093 ± 1.037	5.687 ± 0.020

Fig. 8 In vitro corrosion behavior of samples after immersion: a SEM images of samples immersed in SBF solution for 7 days, b changes in hydrogen evolution during immersion, c pH value, d average corrosion rate immersion for 7 days and for 30 days, e XRD analysis of the T-20 sample after corrosion

Fig. 9 SEM images of corrosion product removal after the samples were immersed in SBF solution for 7 days

Fig. 10 Corrosion mechanism of the core-shell structure in SBF solution: a mechanism of Mg core degradation, b galvanic corrosion between matrix and shell phase, c uniform corrosion of the Zn matrix

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