材料期刊网

通过碳化二亚胺(EDC)改性、二次冻干制备多孔胶原-β-磷酸三钙-硫酸软骨素复合膜材料.通过扫描电镜(SEM)、X射线衍射分析仪(XRD)与原子力显微镜(AFM)考察了组分变化与制备过程中复合材料的微观形貌变化,并进一步利用红外、孔隙率、MTT细胞毒性实验等分析手段对复合材料的结构与性能进行了表征.实验结果表明,当胶原盐酸溶解液pH=2,胶原与β-磷酸三钙质量比为1∶2(m(Col)∶m(β-TCP)=1∶2)时,复合材料中β-TCP晶相保持较好,其与胶原之间的排列结合最为均匀紧密.经EDC改性后,SEM与AFM实验均显示了交联后的胶原束明显变大变粗,以一定的方向紧密地排列在一起.XRD图谱显示复合材料中β-TCP特征衍射峰明显.复合材料的孔径为80～90 μm,三元膜孔隙率为(90.76士1.28)％,大于纯胶原冻干膜(85.88士0.92)％;红外光谱证实β-TCP中的钙离子与Col上的羧基发生了化学键合,AFM显示β-TCP颗粒能与胶原发生直接联结.复合材料的MTT实验结果为1级,是一种潜在的口腔修复膜材料.

The porous collagen-β-tricalcium phosphate-chondroitin sulfate composite membrane was prepared by EDC modification and twice freeze-dried method.The effect of variation of material proportion,pH value and method in materials preparation process on the structure and properties of composite materials were investigated by scanning electron microscope (SEM),X-ray diffraction analyzer (XRD) and atomic force microscope (AFM),FT-IR,porosity measurer,MTT cytotoxicity tester.The results indicated that when the pH value of collagen/HCl solution was 2,the mass ratio of collagen and β-tricalcium phosphate was 1 ∶ 2 (m(Col) ∶ m(β-TCP)=1 ∶ 2),the β-TCP's crystalline phase maintained,the composition was uniform and compact.After EDC modification,the SEM and AFM results showed that the collagen bundles after crosslinking got bigger and thicker obviously,arranged closely in a certain direction.XRD spectrum showed that the characteristic diffraction peaks of β-TCP in composite materials were obvious.The pore size of composite material was about 80-90μm,the porosity of ternary membrane was (90.76±1.28)％,larger than that of collagen membrane (85.88±0.91)％.Infrared spectra confirmed that Ca2+ of β-TCP and carboxyl of Col were chemically bonded.AFM showed that β-TCP particles had a direct connection with collagen.The MTT cytotoxicity levels of composite materials were 1,which was a kind of potential dental restorative material.