Synthesis of Hydroxyapatite Microspheres by Hydro-thermal Method under the Control of Sodium Citrate

doi:10.3724/SP.J.1077.2014.13271

Abstract

Abstract:

Hydroxyapatite (HA) microspheres were prepared by using calcium nitrate tetra hydrate (Ca(NO₃)₂·4H₂O) and diammonium phosphate ((NH₄)₂HPO₄) as the resource of calcium and phosphorus, respectively. During the synthesis, propionamide was used as pH adjusting agent to control the supersaturation of the solution, and trisodium citrate was used as the calcium source relievers to control the morphology of HA. The HA microspheres with high crystallinity, regular morphology and good dispersion were synthesized through hydrothermal method. XRD, FTIR and SEM were used to characterize the product. The effects of starting pH value, the amount of trisodium citrate and reaction temperature on the crystallinity, composition and morphology of HA were investigated. The results show that the optimal condition for uniform HA microspheres was as follows, pH=3, molar ratio of sodium citrate to calcium source at about 1:1.5, and reaction temperature of 180℃.

Key words: hydrothermal method, hydroxyapatite, microspheres, sodium citrate

CLC Number:

TB321

MA Yi-Juan, HAO Li-Jing, DU Shao-Long, ZHAO Na-Ru. Synthesis of Hydroxyapatite Microspheres by Hydro-thermal Method under the Control of Sodium Citrate[J]. Journal of Inorganic Materials, 2014, 29(3): 284-288.

Figures/Tables 7

Fig. 1 XRD patterns of products under varied initial pH values (a) pH=2; (b) pH=3; (c) pH =4; ( d) pH=5 Tick marks below the patterns corresponding to the position of the Bragg reflections of the HA (JCPDS 72-1243)

Fig. 2 FTIR patterns of synthesized products by hydrothermal method under varied initial pH values (a) pH=2; (b) pH=3; (c) pH =4; (d) pH=5

Fig. 3 SEM images of synthesized products by hydrothermal method under varied initial pH values (a) pH=2; (b) pH=3; (c) pH =4; (d) pH=5

Fig. 4 XRD patterns of the products synthesized with varied molar ratios of sodium citrate to calcium source (a) TSC/Ca=1:0.5; (b) TSC/Ca =1:1; (c) TSC/Ca =1:1.5; (d) TSC/Ca =1:3 Tick marks below the patterns correspond to the position of the Bragg reflections of the Earlandite (JCPDS 28-2003) and the hexagonal HA (JCPDS 72-1243)

Fig. 5 SEM images of the products synthesized with varied molar ratios of sodium citrate to calcium source (a) TSC/Ca =1:0.5; (b) TSC/Ca =1:1; (c) TSC/Ca =1:1.5; (d) TSC/Ca =1:3

Fig. 6 XRD patterns of the products synthesized under varied hydrothermal temperatures (a) T=120℃; (b) T =150℃; (c) T =180℃ Tick marks below the patterns correspond to the position of the Bragg reflections of the Earlandite (JCPDS 28-2003) and the hexagonal HA (JCPDS 72-1243)

Fig.7 SEM images of the products synthesized under varied hydrothermal temperatures (a) T=120℃; (b) T=150℃; (c) T=180℃

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