Synthesis and Characterization of Copper-substituted Hydroxyapatite Micrspheres

doi:10.3724/SP.J.1077.2014.13532

Abstract

Abstract:

As the second essential trace element in human body, copper plays vital roles in metabolism and antimicrobial. Therefore, synthesis of copper-substituted hydroxyapatite (Cu-HA) is expected to create bioceramics with improved biological and antimicrobial properties. In this study, Cu-HA was prepared by hydrothermal reactions using Ca(NO₃)₂∙4H₂O, Cu(NO₃)₂∙3H₂O and Na₂HPO₄∙12H₂O. Products were characterized by scanning electron microscope, transmission electron microscope, X-ray diffraction, Fourier transform infrared spectroscope and atomic absorption spectrometry. Results show that copper is incorporated into the HA crystals. Correspondingly, the products retain HA structure but their morphologies transform from ribbons to flower-like microspheres. Moreover, when Cu/(Cu+Ca) (molar ratio) of the reaction solution is greater than 0.05, the thermal stability of the HA product is decreased.

Key words: hydroxyapatite, copper substitution, microspheres, hydrothermal synthesis

CLC Number:

TQ174

XIAO Dong-Qin, WANG Dong-Wei, REN Jun-Chen, DUAN Ke, YAO Ning, LU Xiong, ZHENG Xiao-Tong, WENG Jie. Synthesis and Characterization of Copper-substituted Hydroxyapatite Micrspheres[J]. Journal of Inorganic Materials, 2014, 29(7): 769-775.

Figures/Tables 10

Table 1 Solutions used for hydrothermal preparation of Cu-HA

Solution	Ca(NO₃)₂ /mmol	Cu(NO₃)₂ /mmol	=n(Cu)/ n(Cu+Ca)
S0	3	0	0
S1	2.97	0.03	0.01
S2	2.91	0.09	0.03
S3	2.85	0.15	0.05
S4	2.7	0.3	0.1
S5	2.4	0.6	0.2

Fig. 1 SEM images of Cu-HA prepared by reaction at 150℃ for 3 h in different solutions (a) S0; (b) S1; (c) S2; (d) S3; (e) S4; (f) S5

Fig. 2 TEM images of Cu-HA (S3) prepared by reaction at 150℃ for 3 h

Fig. 3 XRD patterns of Cu-HA prepared by reaction at 150℃ for 3 h in different solutionse

Fig. 4 XRD patterns of Cu-HA (S2, S3, S4 and S5) prepared by reaction at 150℃ for 3 h and subsequently calcinated at 900℃ for 1 h

Fig. 5 FTIR spectra of Cu-HA (S0, S1, S2 and S3) prepared by reaction at 150℃ for 3 h

Table 2 Cu-substitution ratio of Cu-HA

Sample	χ_t (Theoretical)	χ_a (Actual)	R /%
S1	0.01	0.0076	76
S2	0.03	0.0144	48
S3	0.05	0.0155	31

Fig. 6 SEM images of Cu-HA (S3) prepared by reaction at 120℃(a, b), 150℃(c, d) and 200℃(e, f) for 3 h

Fig. 7 XRD patterns of Cu-HA (S3) prepared by reaction at different temperatures for 3 h

Fig. 8 SEM images and XRD patterns of Cu-HA (S3) prepared by reaction at 150℃ for 0.5 h (a), 1 h (b), 2 h (c) and 3 h (d)

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