J. Mater. Sci. Technol. ›› 2020, Vol. 38: 148-158.DOI: 10.1016/j.jmst.2019.03.048
• Research Article • Previous Articles Next Articles
Zhu Huia, Guo Daganga*(), Zang Hangb*(), A.H. Hanaor Dorianc, Yu Senad, Schmidt Franziskac, Xu Keweia
Received:
2018-12-23
Revised:
2019-03-05
Accepted:
2019-03-25
Published:
2020-02-01
Online:
2020-02-10
Contact:
Guo Dagang,Zang Hang
Zhu Hui, Guo Dagang, Zang Hang, A.H. Hanaor Dorian, Yu Sen, Schmidt Franziska, Xu Kewei. Enhancement of hydroxyapatite dissolution through structure modification by Krypton ion irradiation[J]. J. Mater. Sci. Technol., 2020, 38: 148-158.
Fig. 1. (a) 3D surface morphology gradient map of a typical HA coating on a fused silica substrate. (b) Sample fixing setup for ion irradiation. (c) A diagram of irradiation process.
Fig. 2. SRIM simulation of the irradiation induced damage variations and Kr ion distribution with depth. Irradiation on the Cu foil and bulk Cu sample. Pink areas in the figures represent the 100-nm TEM foils and yellow areas represent the 2 μm HA coatings.
Sample label | Displacements-per-atom | Ion fluence |
---|---|---|
S0 | 0 | 0 |
S1 | 0.005 dpa | 1 × 1013 ions/cm2 |
S2 | 0.01 dpa | 2 × 1013 ions/cm2 |
S3 | 0.05 dpa | 1 × 1014 ions/cm2 |
S4 | 0.1 dpa | 2 × 1014 ions/cm2 |
S5 | 0.5 dpa | 1 × 1015 ions/cm2 |
Table 1 Correspondence of dpa to ion fluences.
Sample label | Displacements-per-atom | Ion fluence |
---|---|---|
S0 | 0 | 0 |
S1 | 0.005 dpa | 1 × 1013 ions/cm2 |
S2 | 0.01 dpa | 2 × 1013 ions/cm2 |
S3 | 0.05 dpa | 1 × 1014 ions/cm2 |
S4 | 0.1 dpa | 2 × 1014 ions/cm2 |
S5 | 0.5 dpa | 1 × 1015 ions/cm2 |
Fig. 4. (a) Cavities formation and evolution in the HA nanoparticles after irradiation with 4 MeV Kr17+ ions with increasing irradiation fluence at room temperature. (b) Cavity size variations upon the heavy ion fluence from TEM observations. (c) EDS spectrum taken from S0. (d) EDS spectrum taken from S3.
Fig. 5. Typical TEM images of the HA nanoparticles before and after Kr irradiation. (a) unirradiated, (b) 1 × 1013 ions/cm2 (0.005 dpa) and (c) its inverse fast fourier transform, (d) and (e) 2 × 1013 ions/cm2 (0.01 dpa), (f) 1 × 1014 ions/cm2 (0.05 dpa), (g) 2 × 1014 ions/cm2 (0.1 dpa), (h) 1 × 1015 ions/cm2 (0.5 dpa), (i) SAED patterns of the sampels irradiated with various fluences.
Fig. 6. Raman analysis: Spectra of samples irradiated at different doses are shown (a) over the full range of shifts, and in the shift ranges of (b) 350 to 650 cm-1, (c) 890 to 1000 cm-1, (d) 1000 to 1150 cm-1, (e) 3500 to 3650 cm-1. Decay of this band’s intensity, change of its position, and the increase of its breadth as indicated by FWHMs are plotted as a function of ion fluence in (f), (g) and (h) respectively. (i) the area ratio of the radiation-induced broad ν1b band (950 cm-1) to the ν1 band (962 cm-1).
Fig. 7. XPS O 1s spectra for samples with increasing irradiation dose. (a) unirradiated, (b) 1 × 1013 ions/cm2 (0.005 dpa), (c) 2 × 1013 ions/cm2 (0.01 dpa), (d) 1 × 1014 ions/cm2 (0.05 dpa), (E) 2 × 1014 ions/cm2 (0.1 dpa), (f) 1 × 1015 ions/cm2 (0.5 dpa). In each subfigure, black markers show the data points, the solid red line shows the fitted profile and the two shaded areas show the deconvoluted contributions of the two binding energies.
Fig. 8. (a) Calcium and (b) phosphate ions released in Tris-buffer solution from HA discs irradiated by 4 MeV Kr17+ ions with different fluences, with respect to immersion duration. Insets: enlarged view from 30 min to 8 h immersion. (c) Comparison of the ion release of pristine sample and 0.1 dpa irradiated samples. (d) HRTEM pictures of the pristine and 0.1 dpa irradiated samples after immersion for 1 and 2 weeks. Arrows indicate the dissolution starting points.
Fig. 9. Selected SEM images of cultured specimens ((a)-(f) 1 × 1013 to 1 × 1015 ions/cm2) at 24 h after MC3T3-E1 were seeded on their surfaces; (g) cell adhesion of MC3T3-E1 cells on the specimens at 24 h; (h) cell proliferation after cell seeding for 1, 3 and 7 days. The modified OD values at 3 and 7 days were normalized to those at 1 day. * denote p < 0.05.
Irradiation dose | HA crystal stuructures |
---|---|
0 | Perfect lattice arrangement |
0.005 dpa | Few dislocations and small mottled contrast |
0.01 dpa | Grain boundaries and numerous dislocation lines. Considerable number of disorders |
0.05 dpa | The original single crystal is broken into isolated crystallites with continuous amorphous phase. |
0.1 dpa | Few crystalline regions embedded in the amorphous matrix. Lattice fringe are still visable |
0.5 dpa | Completely amorphous HA particles. |
Table 2 A summary of irradiation damage progression of HA nanoparticles after irradiation.
Irradiation dose | HA crystal stuructures |
---|---|
0 | Perfect lattice arrangement |
0.005 dpa | Few dislocations and small mottled contrast |
0.01 dpa | Grain boundaries and numerous dislocation lines. Considerable number of disorders |
0.05 dpa | The original single crystal is broken into isolated crystallites with continuous amorphous phase. |
0.1 dpa | Few crystalline regions embedded in the amorphous matrix. Lattice fringe are still visable |
0.5 dpa | Completely amorphous HA particles. |
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