J. Mater. Sci. Technol. ›› 2022, Vol. 103: 73-83.DOI: 10.1016/j.jmst.2021.07.006
• Research Article • Previous Articles Next Articles
Kun Lia,1, Luxin Liangb,1, Peng Dua, Zeyun Caia, Tao Xianga, Hiroyasu Kanetakac,d, Hong Wub,*(
), Guoqiang Xiea,e,*()
Received:2021-04-14
Revised:2021-06-22
Accepted:2021-07-03
Published:2022-03-20
Online:2021-08-27
Contact:
Hong Wu,Guoqiang Xie
About author:xieguoqiang@hit.edu.cn (G. Xie).Kun Li, Luxin Liang, Peng Du, Zeyun Cai, Tao Xiang, Hiroyasu Kanetaka, Hong Wu, Guoqiang Xie. Mechanical properties and corrosion resistance of powder metallurgical Mg-Zn-Ca/Fe bulk metal glass composites for biomedical application[J]. J. Mater. Sci. Technol., 2022, 103: 73-83.
Fig. 1. Time-temperature curve for the SPS of Mg66Zn30Ca4/Fe BMG composites.
Fig. 2. Schematic diagram of the preparation process of Mg66Zn30Ca4/Fe BMG composites.
Fig. 3. SEM images of (a) Mg66Zn30Ca4, and Mg66Zn30Ca4 MG composites with different Fe contents before sintering: (b) 5%, (c) 10%, (d) 15%, and (e, f) 20%.
Fig. 4. XRD patterns of Mg66Zn30Ca4 and Mg66Zn30Ca4/Fe BMG composites after sintering.
Fig. 5. SEM micrographs of (a) Mg66Zn30Ca4 BMG and (b, c) Mg66Zn30Ca4/Fe BMG composites after sintering. (d) Mapping result for the element distribution of Mg66Zn30Ca4/Fe BMG composites. (e) The line scan of the interface between Mg66Zn30Ca4 and Fe. (f) The elements concentration of Mg66Zn30Ca4 and the composites.
| Samples | C | O | Mg | Zn | Ca | Fe |
|---|---|---|---|---|---|---|
| Mg66Zn30Ca4 | 1.97 | 1.68 | 34.87 | 55.83 | 5.65 | - |
| 5% Fe | 2.59 | 2.12 | 33.14 | 52.17 | 5.26 | 4.66 |
| 10% Fe | 2.97 | 2.19 | 30.54 | 50.60 | 4.96 | 8.74 |
| 15% Fe | 2.81 | 2.24 | 29.74 | 48.23 | 4.92 | 12.06 |
| 20% Fe | 2.46 | 2.35 | 28.12 | 45.70 | 4.88 | 16.49 |
Table 1 The concentration (wt.%) of elements in Mg66Zn30Ca4 BMG and the composites.
| Samples | C | O | Mg | Zn | Ca | Fe |
|---|---|---|---|---|---|---|
| Mg66Zn30Ca4 | 1.97 | 1.68 | 34.87 | 55.83 | 5.65 | - |
| 5% Fe | 2.59 | 2.12 | 33.14 | 52.17 | 5.26 | 4.66 |
| 10% Fe | 2.97 | 2.19 | 30.54 | 50.60 | 4.96 | 8.74 |
| 15% Fe | 2.81 | 2.24 | 29.74 | 48.23 | 4.92 | 12.06 |
| 20% Fe | 2.46 | 2.35 | 28.12 | 45.70 | 4.88 | 16.49 |
| Sample | C (wt.%) | O (wt.%) |
|---|---|---|
| Mg66Zn30Ca4 | 0.011 | 0.019 |
| 5% Fe | 0.013 | 0.025 |
| 10% Fe | 0.017 | 0.046 |
| 15% Fe | 0.016 | 0.102 |
| 20% Fe | 0.023 | 0.261 |
Table 2 The contents of C and O of Mg66Zn30Ca4 and the composites.
| Sample | C (wt.%) | O (wt.%) |
|---|---|---|
| Mg66Zn30Ca4 | 0.011 | 0.019 |
| 5% Fe | 0.013 | 0.025 |
| 10% Fe | 0.017 | 0.046 |
| 15% Fe | 0.016 | 0.102 |
| 20% Fe | 0.023 | 0.261 |
Fig. 6. (a) Compression properties, (b) Young's modulus and (c) density of Mg66Zn30Ca4 BMG and composites.
Fig. 7. SEM micrographs of compressive fracture of Mg66Zn30Ca4 BMG (a) and Mg66Zn30Ca4/Fe composite (b).
Fig. 8. (a) Open circuit potential and (b) Tafel polarization curves of Mg66Zn30Ca4 BMG and Mg66Zn30Ca4/Fe BMG composites with different contents of Fe.
| Ecorr (V) | Icorr (A/cm2) | |
|---|---|---|
| Mg66Zn30Ca4 | -1.41±0.2 | (2.5±1.2) × 10-5 |
| 5% Fe | -1.34±0.1 | (2.2±2.3) × 10-4 |
| 10% Fe | -1.31±0.1 | (1.2±2.3) × 10-4 |
| 15% Fe | -1.27±0.1 | (1.3±1.2) × 10-4 |
| 20% Fe | -1.22±0.1 | (9.4±2.4) × 10-5 |
Table 3 The corrosion current density and potential of Mg66Zn30Ca4 and composites.
| Ecorr (V) | Icorr (A/cm2) | |
|---|---|---|
| Mg66Zn30Ca4 | -1.41±0.2 | (2.5±1.2) × 10-5 |
| 5% Fe | -1.34±0.1 | (2.2±2.3) × 10-4 |
| 10% Fe | -1.31±0.1 | (1.2±2.3) × 10-4 |
| 15% Fe | -1.27±0.1 | (1.3±1.2) × 10-4 |
| 20% Fe | -1.22±0.1 | (9.4±2.4) × 10-5 |
Fig. 9. Nyquist plots of Mg66Zn30Ca4 and composite (with 20% content of Fe); Equivalent circuit used to model was inserted.
Fig. 10. Corrosion rate of Mg66Zn30Ca4 BMG after immersion in Hank's solution for 7 days and composite after immersion in Hank's solution for 14 days.
Fig. 11. Surface morphology of Mg66Zn30Ca4 and composites after immersion in Hank's solution for 6 days.
Fig. 12. SEM images of Mg66Zn30Ca4 BMG (a, b) and Mg66Zn30Ca4/Fe composites (c, d) after immersion in Hank's solution for 7 days.
Fig. 13. XRD patterns of Mg66Zn30Ca4/Fe BMG composites after immersion in Hank's solution for 2 weeks.
Fig. 14. The compressive stress and Young's modulus of composites after 5 days of immersion.
| Mg2+ | Zn2+ | Ca2+ | Fe3+ | pH value | |
|---|---|---|---|---|---|
| Complete medium | 19.2±1.2 | - | 38.0±1.6 | - | 7.40±0.02 |
| Mg66Zn30Ca4 | 2119.3±156.2 | 22.6±4.0 | 46.8±4.6 | - | 8.36±0.04 |
| Mg66Zn30Ca4/Fe | 842.5±56.4 | 75.4±8.1 | 58.9±5.2 | 0.9±0.2 | 8.24±0.03 |
Table 4 Concentrations (mg/L) of Mg2+, Zn2+, Ca2+, Fe3+ and pH values in supernatants after immersing different specimens for 72 hours.
| Mg2+ | Zn2+ | Ca2+ | Fe3+ | pH value | |
|---|---|---|---|---|---|
| Complete medium | 19.2±1.2 | - | 38.0±1.6 | - | 7.40±0.02 |
| Mg66Zn30Ca4 | 2119.3±156.2 | 22.6±4.0 | 46.8±4.6 | - | 8.36±0.04 |
| Mg66Zn30Ca4/Fe | 842.5±56.4 | 75.4±8.1 | 58.9±5.2 | 0.9±0.2 | 8.24±0.03 |
Fig. 15. Cell proliferation measured by (a) CCK-8 and (b) live-cell staining assay after culturing RAW 264.7 macrophages in various EMs for 1 day, 3 days and 5 days. *p<0.05, compared to the control; #p<0.05, compared to the Mg66Zn30Ca4/Fe EM × 6 group.
| Mg2+ | Zn2+ | Ca2+ | Fe3+ | |
|---|---|---|---|---|
| Mg66Zn30Ca4 EM × 6 | 369.2 | 3.8 | 39.5 | - |
| Mg66Zn30Ca4EM × 10 | 229.2 | 2.3 | 38.9 | - |
| Mg66Zn30Ca4/FeEM × 6 | 156.4 | 12.6 | 41.5 | 0.15 |
| Mg66Zn30Ca4/Fe EM × 10 | 101.5 | 7.5 | 40.9 | 0.09 |
Table 5 Concentrations (mg/L) of ions in the various EMs after diluting the supernatants by 6 or 10 times.
| Mg2+ | Zn2+ | Ca2+ | Fe3+ | |
|---|---|---|---|---|
| Mg66Zn30Ca4 EM × 6 | 369.2 | 3.8 | 39.5 | - |
| Mg66Zn30Ca4EM × 10 | 229.2 | 2.3 | 38.9 | - |
| Mg66Zn30Ca4/FeEM × 6 | 156.4 | 12.6 | 41.5 | 0.15 |
| Mg66Zn30Ca4/Fe EM × 10 | 101.5 | 7.5 | 40.9 | 0.09 |
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