Acta Metallurgica Sinica (English Letters) ›› 2022, Vol. 35 ›› Issue (2): 304-316.DOI: 10.1007/s40195-021-01248-8
Special Issue: 腐蚀-2 2022
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Sharafadeen Kunle Kolawole1,2,3, Ling Ren2(
), Muhammad Ali Siddiqui1,2, Ihsan Ullah1,2, Hai Wang2, Shuyuan Zhang2, Ji Zhang2, Ke Yang2(
)
Received:2020-12-16
Revised:2021-01-19
Accepted:2021-04-06
Online:2022-02-10
Published:2021-05-08
Contact:
Ling Ren,Ke Yang
About author:Ke Yang, kyang@imr.ac.cnSharafadeen Kunle Kolawole, Ling Ren, Muhammad Ali Siddiqui, Ihsan Ullah, Hai Wang, Shuyuan Zhang, Ji Zhang, Ke Yang. Optimized Mechanical Properties, Corrosion Resistance and Bactericidal Ability of Ti-15Zr-xCu Biomedical Alloys During Aging Treatment[J]. Acta Metallurgica Sinica (English Letters), 2022, 35(2): 304-316.
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| Constituent element | TZ (wt%) | TZC-3 (wt%) | TZC-5 (wt%) | TZC-7 (wt%) |
|---|---|---|---|---|
| Ti | Bal | Bal | Bal | Bal |
| Zr | 14.90 | 15.20 | 14.70 | 15.05 |
| Cu | 0.03 | 2.89 | 5.02 | 6.97 |
| Fe | 0.02 | 0.05 | 0.06 | 0.02 |
| C | 0.04 | 0.03 | 0.05 | 0.05 |
| O | 0.06 | 0.07 | 0.09 | 0.07 |
| N | 0.006 | 0.004 | 0.05 | 0.009 |
| H | 0.003 | 0.003 | 0.003 | 0.002 |
Table 1 Chemical compositions of the Ti-15Zr alloy and Ti-15Zr-xCu alloys
| Constituent element | TZ (wt%) | TZC-3 (wt%) | TZC-5 (wt%) | TZC-7 (wt%) |
|---|---|---|---|---|
| Ti | Bal | Bal | Bal | Bal |
| Zr | 14.90 | 15.20 | 14.70 | 15.05 |
| Cu | 0.03 | 2.89 | 5.02 | 6.97 |
| Fe | 0.02 | 0.05 | 0.06 | 0.02 |
| C | 0.04 | 0.03 | 0.05 | 0.05 |
| O | 0.06 | 0.07 | 0.09 | 0.07 |
| N | 0.006 | 0.004 | 0.05 | 0.009 |
| H | 0.003 | 0.003 | 0.003 | 0.002 |
| Alloy composition (wt%) | Coined nomenclature | Heat treatment conditions | Coined nomenclature |
|---|---|---|---|
| Ti-15Zr | TZ | Solution treatment at 1050 °C for 2 h and water-quenched | ST |
| Ti-15Zr-3Cu | TZC-3 | Solution-treated at 1050 °C for 2 h, water-quenched + aging at 450 °C for 10 h, then air-cooled | STA 450-10 |
| Ti-15Zr-5Cu | TZC-5 | Solution-treated at 1050 °C for 2 h, water-quenched + aging at 540 °C for 6 h, then air-cooled | STA 540-6 |
| Ti-15Zr-7Cu | TZC-7 | Solution-treated at 1050 °C for 2 h, water-quenched + aging at 660 °C for 4 h, then air-cooled | STA 660-4 |
Table 2 Nomenclatures for the composition of different alloys and heat treatment conditions
| Alloy composition (wt%) | Coined nomenclature | Heat treatment conditions | Coined nomenclature |
|---|---|---|---|
| Ti-15Zr | TZ | Solution treatment at 1050 °C for 2 h and water-quenched | ST |
| Ti-15Zr-3Cu | TZC-3 | Solution-treated at 1050 °C for 2 h, water-quenched + aging at 450 °C for 10 h, then air-cooled | STA 450-10 |
| Ti-15Zr-5Cu | TZC-5 | Solution-treated at 1050 °C for 2 h, water-quenched + aging at 540 °C for 6 h, then air-cooled | STA 540-6 |
| Ti-15Zr-7Cu | TZC-7 | Solution-treated at 1050 °C for 2 h, water-quenched + aging at 660 °C for 4 h, then air-cooled | STA 660-4 |
| Alloys | Constituent phase(s)/element(s) present | Ti (wt%) | Zr (wt%) | Cu (wt%) | Relative composition Ti2Cu (wt%) | Relative composition Zr2Cu (wt%) | Relative composition Zr7Cu10 (wt%) |
|---|---|---|---|---|---|---|---|
| 0-450-10 | α-(Ti, Zr) | 70.90 | 28.70 | 0.30 | - | - | - |
| 3-450-10 | α-(Ti, Zr) + Ti2Cu | 63.70 | 32.30 | 0.50 | 3.40 | - | - |
| 5-450-10 | Zr7Cu10 + Ti2Cu, α + β—(Ti) | 57.10 | 14.40 | 17 | - | - | 11.40 |
| 7-450-10 | Zr7Cu10 + Ti2Cu, α + β—(Ti) | 52.90 | 12.30 | 3.60 | 21.30 | - | 9.80 |
| 0-540-6 | α-(Ti, Zr) | 81.50 | 18.30 | 0.10 | - | - | - |
| 3-540-6 | Cu + Ti2Cu, α + β—(Ti) | 60.20 | 6.30 | 10.20 | 23.10 | - | - |
| 5-540-6 | Zr2Cu + Ti2Cu, α + β—(Ti) | 56 | 12.20 | 10.10 | 10.90 | 10.70 | - |
| 7-540-6 | Zr2Cu + Ti2Cu, α + β—(Ti) | 55.30 | 12.50 | 12 | 11.40 | 8.70 | - |
| 0-660-4 | α-(Ti, Zr) | 79.40 | 20.10 | 0.40 | - | - | - |
| 3-660-4 | Ti2Cu, α + β-(Ti) | 50.80 | 11.40 | 17.10 | 20.60 | - | - |
| 5-660-4 | Zr2Cu + Ti2Cu, α + β—(Ti) | 51.60 | 9.80 | 10.40 | 18.70 | 9.40 | - |
| 7-660-4 | Zr2Cu + Ti2Cu, α + β—(Ti) | 50.70 | 11.10 | 11.50 | 13.80 | 10.60 | 2.30 |
Table 3 Relative composition of constituent phases/elements present in alloys after STA at different temperatures for different time
| Alloys | Constituent phase(s)/element(s) present | Ti (wt%) | Zr (wt%) | Cu (wt%) | Relative composition Ti2Cu (wt%) | Relative composition Zr2Cu (wt%) | Relative composition Zr7Cu10 (wt%) |
|---|---|---|---|---|---|---|---|
| 0-450-10 | α-(Ti, Zr) | 70.90 | 28.70 | 0.30 | - | - | - |
| 3-450-10 | α-(Ti, Zr) + Ti2Cu | 63.70 | 32.30 | 0.50 | 3.40 | - | - |
| 5-450-10 | Zr7Cu10 + Ti2Cu, α + β—(Ti) | 57.10 | 14.40 | 17 | - | - | 11.40 |
| 7-450-10 | Zr7Cu10 + Ti2Cu, α + β—(Ti) | 52.90 | 12.30 | 3.60 | 21.30 | - | 9.80 |
| 0-540-6 | α-(Ti, Zr) | 81.50 | 18.30 | 0.10 | - | - | - |
| 3-540-6 | Cu + Ti2Cu, α + β—(Ti) | 60.20 | 6.30 | 10.20 | 23.10 | - | - |
| 5-540-6 | Zr2Cu + Ti2Cu, α + β—(Ti) | 56 | 12.20 | 10.10 | 10.90 | 10.70 | - |
| 7-540-6 | Zr2Cu + Ti2Cu, α + β—(Ti) | 55.30 | 12.50 | 12 | 11.40 | 8.70 | - |
| 0-660-4 | α-(Ti, Zr) | 79.40 | 20.10 | 0.40 | - | - | - |
| 3-660-4 | Ti2Cu, α + β-(Ti) | 50.80 | 11.40 | 17.10 | 20.60 | - | - |
| 5-660-4 | Zr2Cu + Ti2Cu, α + β—(Ti) | 51.60 | 9.80 | 10.40 | 18.70 | 9.40 | - |
| 7-660-4 | Zr2Cu + Ti2Cu, α + β—(Ti) | 50.70 | 11.10 | 11.50 | 13.80 | 10.60 | 2.30 |
Fig. 4 SEM images of TZ, TZC-3, TZC-5 and TZC-7 alloys solution-treated and aged (STA) at a-d 450 °C for 10 h, e-h 540 °C for 6 h, and i-l 660 °C for 4 h, respectively
Fig. 5 X-ray diffractograms for the solution-treated and aged TZ, TZC-3, TZC-5, TZC-7 alloys at a 450 °C for 10 h, b 540 °C for 6 h, and c 660 °C for 4 h, respectively
Fig. 6 Ultimate tensile strengths, yield strengths and elongations of the TZ and TZC alloys: a solution-treated at 1050 °C, b solution-treated and then aged at 450 °C for 10 h, c solution-treated and then aged at 540 °C for 6 h, and d solution-treated and then aged at 660 °C for 4 h
Fig. 7 Hardness values of the ST and STA alloys at various conditions. Inset: representative indentation of alloys’ microstructures at ST and STA conditions showing martensite-like parallel and shiny marks for the ST and dimple-like dull marks for the STA alloys, respectively
Fig. 8 Representative photographs of the typical S. aureus colonization behavior on the various solution-treated and then aged (STA), a TZ, b TZC-3, c TZC-5, d TZC-7, e blank control at 450 °C for10 h, f TZ, g TZC-3, h TZC-5, i TZC-7, j blank control at 540 °C for 6 h, k TZ, l TZC-3, m TZC-5, n TZC-7, p blank control at 660 °C for 4 h, and q the respective antibacterial rates of the corresponding alloys at different conditions
Fig. 9 Potentiodynamic polarization curves for the solution-treated and aged TZ, TZC-3, TZC-5, TZC-7 alloys at a 450 °C for 10 h; b 540 °C for 6 h, and c 660 °C for 4 h, respectively
Fig. 10 Concentration of Cu ions released (in mg/L) from differently aged TZ, TZC-3, TZC-5 and TZC-7 alloys over a 35-day period showing that the minimum lethal dosage threshold (LD 50) is not crossed
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