J. Mater. Sci. Technol. ›› 2020, Vol. 50: 31-43.DOI: 10.1016/j.jmst.2020.03.003
• Research Article • Previous Articles Next Articles
Sharafadeen Kunle Kolawolea,b,4, Wang Haib, Shuyuan Zhangb, Ziqing Sunb, Muhammad Ali Siddiquia,b, Ihsan Ullaha,b, Wei Songb, Frank Wittec, Ke Yangb,*()
Received:
2019-12-02
Revised:
2020-01-09
Accepted:
2020-01-22
Published:
2020-08-01
Online:
2020-08-10
Contact:
Ke Yang
Sharafadeen Kunle Kolawole, Wang Hai, Shuyuan Zhang, Ziqing Sun, Muhammad Ali Siddiqui, Ihsan Ullah, Wei Song, Frank Witte, Ke Yang. Preliminary study of microstructure, mechanical properties and corrosion resistance of antibacterial Ti-15Zr-xCu alloy for dental application[J]. J. Mater. Sci. Technol., 2020, 50: 31-43.
Element (components i) | Bo | Md (eV) |
---|---|---|
Ti | 2.790 | 2.447 |
Zr | 3.086 | 2.934 |
Cu | 2.114 | 0.567 |
Table 1 Bo and Md values for various alloying elements in bcc Ti, adapted from Abdel Hady et al. [31].
Element (components i) | Bo | Md (eV) |
---|---|---|
Ti | 2.790 | 2.447 |
Zr | 3.086 | 2.934 |
Cu | 2.114 | 0.567 |
Fig. 1. Map of phase stability index for the new alloys based on Bo$\bar{1}$ and Md$\bar{1}$ for 3 wt.% Cu (oval), 5 wt.% Cu (star) and 7 wt.% Cu (rectangle), as adapted from Abdel-Hady et al. [31].
Element | T-15Z (wt.%) | TZC-3 (wt.%) | TZC-5 (wt.%) | TZC-7 (wt.%) |
---|---|---|---|---|
Ti | Bal. | Bal. | Bal. | Bal. |
Zr | 15.20 | 14.50 | 14.20 | 14.30 |
Cu | 0.01 | 3.00 | 4.95 | 6.95 |
Fe | 0.04 | 0.04 | 0.04 | 0.05 |
C | 0.05 | 0.04 | 0.03 | 0.04 |
O | 0.07 | 0.08 | 0.10 | 0.09 |
N | 0.004 | 0.007 | 0.03 | 0.007 |
H | 0.002 | 0.002 | 0.003 | 0.002 |
Table 2 Chemical composition of the Ti-15Zr-xCu alloys.
Element | T-15Z (wt.%) | TZC-3 (wt.%) | TZC-5 (wt.%) | TZC-7 (wt.%) |
---|---|---|---|---|
Ti | Bal. | Bal. | Bal. | Bal. |
Zr | 15.20 | 14.50 | 14.20 | 14.30 |
Cu | 0.01 | 3.00 | 4.95 | 6.95 |
Fe | 0.04 | 0.04 | 0.04 | 0.05 |
C | 0.05 | 0.04 | 0.03 | 0.04 |
O | 0.07 | 0.08 | 0.10 | 0.09 |
N | 0.004 | 0.007 | 0.03 | 0.007 |
H | 0.002 | 0.002 | 0.003 | 0.002 |
Fig. 3. Differential scanning calorimetry curves of T-15Z (a), TZC-3 (b), TZC-5 (c), TZC-7 (d) which show that Cu additions led to lowered BTT and precipitation of other phases.
Fig. 5. SEM microstructures for (a) TZC-7A, (b) TZC-5A, (c) TZC-3A, (d) T-15ZA; TEM microstructures and their corresponding selected area diffraction patterns (SADP) for (e) TZC-7A, (f) TZC-5A, (g) TZC-3A, (h) T-15ZA; EDS elemental spectrums for (ai) Point A (Ti2Cu) in TZC-7A, (aii) Point B (Zr2Cu) in TZC-7A, (bi) Point C (Ti2Cu) in TZC-5A, (bii) Point D (Zr2Cu) in TZC-5A and (ci) Area E (Ti2Cu) in TZC-3A.
Alloys | Locations | Constituent phase | Ti (wt.%) | Zr (wt.%) | Cu (wt.%) |
---|---|---|---|---|---|
TZC-3A | Area A | Ti2Cu | 67.2 | 3.3 | 29.5 |
TZC-5A | Point A | Ti2Cu | 64.4 | 3.9 | 31.7 |
Point B | Zr2Cu | 48.6 | 34.1 | 17.3 | |
1 | α | 89.4 | 7.4 | 3.2 | |
2 | β | 76.3 | 15.7 | 8.0 | |
TZC-7A | Point A | Ti2Cu | 66.0 | 0.6 | 33.4 |
Point B | Zr2Cu | 54.5 | 33.1 | 12.4 | |
1 | α | 70.8 | 21.4 | 7.8 | |
2 | β | 80.3 | 4.5 | 15.2 |
Table 3 TEM-EDS chemical position for the phases present in the FC Ti-15Zr-xCu alloys.
Alloys | Locations | Constituent phase | Ti (wt.%) | Zr (wt.%) | Cu (wt.%) |
---|---|---|---|---|---|
TZC-3A | Area A | Ti2Cu | 67.2 | 3.3 | 29.5 |
TZC-5A | Point A | Ti2Cu | 64.4 | 3.9 | 31.7 |
Point B | Zr2Cu | 48.6 | 34.1 | 17.3 | |
1 | α | 89.4 | 7.4 | 3.2 | |
2 | β | 76.3 | 15.7 | 8.0 | |
TZC-7A | Point A | Ti2Cu | 66.0 | 0.6 | 33.4 |
Point B | Zr2Cu | 54.5 | 33.1 | 12.4 | |
1 | α | 70.8 | 21.4 | 7.8 | |
2 | β | 80.3 | 4.5 | 15.2 |
Alloys | Relative density (%) | Young’s modulus (GPa) |
---|---|---|
T-15Z | 99.58 ± 0.14 | 110 |
TZC-3 | 99.92 ± 0.05 | 108 |
TZC-5 | 99.60 ± 0.20 | 107 |
TZC-7 | 99.59 ± 0.38 | 103 |
Table 4 Values of relative density and Young’s modulus for the Ti-15Zr-xCu based alloys.
Alloys | Relative density (%) | Young’s modulus (GPa) |
---|---|---|
T-15Z | 99.58 ± 0.14 | 110 |
TZC-3 | 99.92 ± 0.05 | 108 |
TZC-5 | 99.60 ± 0.20 | 107 |
TZC-7 | 99.59 ± 0.38 | 103 |
Fig. 6. Mechanical properties for the T-15ZA, TZC-3A, TZC-5A and TZC-7A alloys showing the trend of increase in strengths and hardness as the Cu contents increased without significant loss in ductility.
Fig. 7. Typical photos (a) and representative graph (b) of colonization by E. coli and S. aureus at 24 h which show a high number of bacteria colonies attached to the T-15ZA alloys and substantially reduced number on the TZC-7A, TZC-3A and TZC-5A alloys.
Fig. 8. Confocal laser scanning microscopy images of (a) TZC-7A; (b) TZC-5A; (c) TZC-3A; (d) T-15ZA showing reduced film thickness and dead biofilms (in red) on the TZC-7A, TZC-3A and TZC-5A alloys and numerous live biofilms (green) on the T-15ZA alloy.
RGR (%) | Grade | Evaluation criterion | RGR (%) | Grade | Evaluation criterion |
---|---|---|---|---|---|
≥100 | 0 | Non-cytotoxic | 25-49 | 3 | Cytotoxic |
75-99 | 1 | Non-cytotoxic | 1-24 | 4 | Cytotoxic |
50-74 | 2 | - | 0 | 5 | Cytotoxic |
Table 5 Classification of cell toxicity, as adapted from Liu et al. [15].
RGR (%) | Grade | Evaluation criterion | RGR (%) | Grade | Evaluation criterion |
---|---|---|---|---|---|
≥100 | 0 | Non-cytotoxic | 25-49 | 3 | Cytotoxic |
75-99 | 1 | Non-cytotoxic | 1-24 | 4 | Cytotoxic |
50-74 | 2 | - | 0 | 5 | Cytotoxic |
Fig. 10. Merged fluorescent images of MC3T3-E1 cultured on the surfaces of the four alloy samples stained with DAPI (blue) for nucleus and Rhodamine Phalloidin (red) for cytoskeleton; upper cells: 4 h; lower cells: 24 h. The TZC-7A alloy displays the highest number of cell attachment and growth at 24 h.
Fig. 13. Corresponding contact angle graphs and water droplet images of (a) T-15ZA, (b) TZC-3A, (c) TZC-5A and (d) TZC-7A showing all samples possess hydrophilic surfaces (< 90°) after FC.
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