[Preparation and properties of silica/hydroxyapatite whiskers porous ceramics scaffold].

Objective: To investigate the preparation and properties of the novel silica (SiO 2)/hydroxyapatite (HAP) whiskers porous ceramics scaffold. Methods: The HAP whiskers were modified by the SiO 2 microspheres using the Stöber method. Three types of SiO 2/HAP whiskers were fabricated under different factors (for the No.1 samples, the content of tetraethoxysilane, stirring time, calcination temperature, and soaking time were 10 mL, 12 hours, 560℃, and 0.5 hours, respectively; and in the No.2 samples, those were 15 mL, 24 hours, 650℃, and 2 hours, respectively; while those in the No.3 samples were 20 mL, 48 hours, 750℃, and 4 hours, respectively). The phase and morphology of the self-made HAP whisker and 3 types of SiO 2/HAP whiskers were detected by the X-ray diffraction analysis and scanning electron microscopy. Taken the self-made HAP whisker and 3 types of SiO 2/HAP whiskers as raw materials, various porous ceramic materials were prepared using the mechanical foaming method combined with extrusion molding method, and the low-temperature heat treatment. The pore structure of porous ceramics was observed by scanning electron microscopy. Its porosity and pore size distribution were measured. And further the axial compressive strength was measured, and the biodegradability was detected by simulated body fluid. Cell counting kit 8 method was used to conduct cytotoxicity experiments on the extract of porous ceramics. Results: The SiO 2 microspheres modified HAP whiskers and its porous ceramic materials were prepared successfully, respectively. In the SiO 2/HAP whiskers, the amorphous SiO 2 microspheres with a diameter of 200 nm, uniform distribution and good adhesion were attached to the surface of the whiskers, and the number of microspheres was controllable. The apparent porosity of the porous ceramic scaffold was about 78%, and its pore structure was composed of neatly arranged longitudinal through-holes and a large number of micro/nano through-holes. Compared with HAP whisker porous ceramic, the axial compressive strength of the SiO 2/HAP whisker porous ceramics could reach 1.0 MPa, which increased the strength by nearly 4 times. Among them, the axial compressive strength of the No.2 SiO 2/HAP whisker porous ceramic was the highest. The SiO 2 microspheres attached to the surface of the whiskers could provide sites for the deposition of apatite. With the content of SiO 2 microspheres increased, the deposition rate of apatite accelerated. The cytotoxicity level of the prepared porous ceramics ranged from 0 to 1, without cytotoxicity. Conclusion: SiO 2/HAP whisker porous ceramics have good biological activity, high porosity, three-dimensional complex pore structure, good axial compressive strength, and no cytotoxicity, which make it a promising scaffold material for bone tissue engineering.

Crystal Structure and Bond-Valence Investigation of Nitrogen-Stabilized LiAl5O8 Spinels.

An in-depth insight into the effect of nitrogen substitution on structural stabilization is important for the design of new spinel-type oxynitride materials with tailored properties. In this work, the crystal structures of ordered and disordered LiAl5O8 obtained by slow cooling and rapid quenching, respectively, were analyzed by a X-ray diffraction (XRD) Rietveld refinement and OccQP program. The variation in the bonding state of atoms in the two compounds was explored by the bond valence model, which revealed that the instability of spinel-type LiAl5O8 crystal structure at room temperature is mainly due to the severe under-bonding of the tetrahedrally coordinated Al cations. With the partial substitution of oxygen with nitrogen in LiAl5O8, a series of the nitrogen-stabilized spinel LiyAl(16+x-y)/3O8-xNx (0 < x < 0.5, 0 < y < 1) was successfully prepared. The crystal structures were systematically investigated by the powder XRD structural refinement combined with 7Li and 27Al magic-angle spinning nuclear magnetic resonance. All the Li+ ions entered the octahedra, while the Al resonances may be composed of multiple non-equivalent Al sites. The structural stability of spinel LiyAl(16+x-y)/3O8-xNx at ambient temperature was attributed to the cationic vacancies and high valence generated by the N ions, which alleviated the under-bonding state of the tetrahedral Al-O bond. This work provides a new perspective for understanding the composition-structure relationship in spinel compounds with multiple disorders.