Calcium Phosphate Cement Reinforced by Nanocrystalline Cellulose

doi:10.15541/jim20140385

Abstract

Abstract:

The aim of this study is to investigate the effect of nanocrystalline cellulose (NCC) with favorable mechanical properties on the compressive strength of calcium phosphate cement (CPC). Compressive test, Gilmore needle test, X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) were used to analyze the physicochemical properties of CPC influenced by different contents of NCC. Scanning electron microscope (SEM) and fluorescence microscope were used to observe the morphologies of CPC and the dispersity of labeled-NCC in CPC, respectively. NCC significantly increased the compressive strength of CPC up to about 27 MPa when the content of NCC was 2%. Setting times of CPC were prolonged with increased NCC, but still met the clinical requirements when the content of NCC was not more than 2%. XRD and XPS indicated that the combination of NCC with Ca²⁺ could form unstable coordination compound and NCC promoted the dissolution and conversion of dicalcium phosphate dehydrate (DCPD) and CaCO₃. SEM showed that CPC became denser with fewer pores and cracks by addition of NCC. Fluorescence microscope demonstrated the homogeneous dispersion of labeled-NCC in CPC.

Key words: calcium phosphate cement, nanocrystalline cellulose, compressive strength, dispersity

CLC Number:

ZHAO Jun-Sheng, QU Shu-Xin, HUANG Ping, LIU Zong-Guang, WANG Shi-Wen, WENG Jie. Calcium Phosphate Cement Reinforced by Nanocrystalline Cellulose[J]. Journal of Inorganic Materials, 2015, 30(3): 318-324.

Figures/Tables 10

Fig. 1 Compressive strength of CPC, 2 %NCC-CPC and 4 %NCC-CPC after setting for 24 h (n=6, *p<0.05, **p<0.01) (a) and the typical stress-strain curves (b)

Fig. 2 Initial and final setting times of CPC, 2% NCC-CPC and 4% NCC-CPC (n=3, *p<0.05, **p<0.01)

Fig. 3 XRD patterns of CPC, 2% NCC-CPC and 4% NCC-CPC (a) and the ratio of the primary diffraction maximum of DCPD and CaCO3 of each CPC sample (Ix) to that of CPC (I0) (b)

Table 1 The binding energy of C1s, O1s and Ca2p core levels from CPC and 2% NCC-CPC

Elements and functional groups		Binding energy/eV
Elements and functional groups		CPC	2% NCC-CPC
C1s	C-C、C-H C-O/C=O C-C/C-O-C	284.8 286.5/288.8 -	284.8 - 286.1/288.3
O1s	P=O P-OH/H₂O C-OH/C-O-C	531.2 532.5 -	531.4 - 532.8
Ca2p	Ca2p_3/2 Ca2p_1/2	351.0 347.3	351.1 347.6

Fig. 4 Chemical structure of NCC DP represents the degree of polymerization

Fig. 5 XPS spectra of CPC and 2% NCC-CPC after setting for 24 h (a) Survey; (b) C1s; (c) O1s; (d) Ca2p

Fig. 6 SEM images of the cross-sections of CPC (a1, a2), 2% NCC-CPC (b1, b2) and 4% NCC-CPC (c1, c2) after setting for 24 h

Fig. 7 Schematic diagram of NCC promoting the setting of CPC by coordination with Ca2+

Fig. 8 TEM image of NCC

Fig. 9 Fluorescence micrographs of NCC labeled by 7-amino-4-methyl coumarin (AMC) that evenly distributed in CPC (a) 2% NCC-CPC; (b) 2% NCC-AMC-CPC; (c) 4% NCC-AMC-CPC

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