骨修复用球状硫酸钙基复合材料制备及其性能研究

发布时间：2018-01-28 17:41

本文关键词： 硫酸钙掺锶β-磷酸三钙复合小球堆垛成型多孔支架　出处：《昆明理工大学》2017年硕士论文　论文类型：学位论文

【摘要】：生物陶瓷材料由于具有良好的生物相容性、生物降解性、骨传导性和骨诱导性等,常被用于修复骨组织缺损、替代失去功能或衰竭的组织、器官的部分或全部。而硫酸钙、磷酸钙类材料是目前应用最为广泛的骨修复用生物陶瓷材料。本文所研究的硫酸钙/掺锶β-TCP复合材料比单一材料在生物活性、降解性等方面具有更多的优势,具有更广泛的应用前景。本文采用搅拌喷雾干燥法成功制备出硫酸钙/掺锶β-TCP复合小球;为了提高复合材料的性能,随后,分别用二氧化硅、明胶、羧甲基纤维素钠与制备的复合小球进行复合,得到了(SiO_2、明胶和羧甲基纤维素钠)/硫酸钙/掺锶β-TCP复合多孔生物支架,并对其进行成分、结构和性能等方面的分析。本文进行了以下研究:以碳酸钙(CaCO_3、硝酸锶(Sr(NO_3)_2)、磷酸(H3PO_4)为原料,用沉淀法制备了掺锶β-磷酸三钙粉体。该粉体中β-TCP为主相占86.7%;该粉体的粒径大小主要分布在10μm～100μm范围内,球磨后粉体粒径为0.5μm～10μm,掺锶量对粉体粒度大小没有较大的影响;锶掺入β-TCP后二者形成了置换固溶体,但掺锶量对晶体结构影响不大。由粉体细胞毒性实验结果可知,该粉体无细胞毒性。采用搅拌喷雾干燥法制备硫酸钙/掺锶β-TCP的复合小球。通过正交试验设计筛选出制备复合小球的最佳工艺方案,即:当CaSO_4粉末添加量、粘接剂的浓度、掺锶β-TCP浓度和掺锶β-TCP所占CaSO_4粉末添加量的比例分别为2.5g,10 wt%,10 wt%和30wt%时,可制备出造球率达75%左右,粒径在0.95-1.35mm之间的复合小球颗粒。细胞毒性结果表明,该颗粒细胞毒性为0级或1级,即无细胞毒性。采用硅胶、明胶和羧甲基纤维素钠三种物质,通过堆垛聚集的方法制备出多孔(SiO_2、明胶和羧甲基纤维素钠)/复合小球生物支架。研究结果表明:三种复合支架的孔隙率均分布在60%左右;三种复合支架都具有不规则的孔洞结构,小球与小球之间形成的孔隙尺寸在0.2-1.Omm之间,SiO_2/复合小球生物支架孔径主要分布在100-300μm;明胶/复合小球生物支架孔径主要分布在100-500μm;羧甲基纤维素钠/复合小球生物支架孔径主要分布在50-300μm。SiO_2/复合小球生物支架的平均抗压强度约为0.1Mpa,明胶/复合小球生物支架的平均抗压强度达到6.3Mpa,羧甲基纤维素钠/复合小球生物支架的平均抗压强度为0.7Mpa;体外生物降解实验发现,三种支架浸泡于SBF的过程中均有磷灰石的沉积,说明其具有良好的生物活性。其中,明胶/复合小球生物支架的降解周期最长,在本实验的80天周期内仍未完全降解,羧甲基纤维素钠/复合小球生物支架的降解周期较短,约为40天,SiO_2/复合小球生物支架在本实验的80天左右基本降解完全。三种复合支架细胞毒性为0级或1级,即无细胞毒性。
[Abstract]:Because of its good biocompatibility, biodegradability, bone conductivity and bone inductivity, bioceramic materials are often used to repair bone defects and replace the tissues with loss of function or failure. Part or all of the organ. And calcium sulfate. Calcium phosphate is the most widely used bioceramic material for bone repair at present. The calcium sulfate / strontium doped 尾 -TCP composite is more bioactive than a single material in this paper. In this paper, calcium sulfate / strontium doped 尾 -TCP composite pellets were successfully prepared by agitation spray drying method. In order to improve the properties of the composites, SiO2 was prepared by using silica, gelatin and sodium carboxymethyl cellulose respectively. Gelatin and carboxymethyl cellulose sodium / calcium sulfate / strontium 尾 -TCP composite porous scaffolds, and their composition. Analysis of structure and properties. The following studies have been carried out in this paper: calcium carbonate Caco _ 3s _ 3, strontium nitrate Srno _ 3s _ 3s _ 2s _ 2, phosphate _ (H _ 3PO _ 4) as raw materials. Sr-doped 尾 -tricalcium phosphate powder was prepared by precipitation method. The particle size of the powder is mainly distributed in the range of 10 渭 m ~ 100 渭 m, and the particle size is 0.5 渭 m ~ (10 渭 m) after ball milling. After strontium was doped with 尾 -TCP, the substitution solid solution was formed, but the content of strontium had little effect on the crystal structure. The powder has no cytotoxicity. Calcium sulfate / strontium doped 尾 -TCP composite pellets were prepared by agitation spray drying method. That is, when the amount of CaSO_4 powder, the concentration of binder, the concentration of strontium 尾 -TCP and the proportion of strontium 尾 -TCP to CaSO_4 powder are 2.5g / 10wt% respectively. The composite pellets with pelletizing rate of about 75% and diameter of 0.95-1.35mm could be prepared at 10 wt% and 30wt%. The cytotoxicity results showed. The cytotoxicity of the granulosa is grade 0 or grade 1, that is, there is no cytotoxicity. Using silica gel, gelatin and sodium carboxymethyl cellulose, porous sio _ s _ 2 was prepared by stacking and aggregating. The results showed that the porosity of the three composite scaffolds was about 60%; The three kinds of composite scaffolds all have irregular pore structure, and the pore size between the small sphere and the small sphere is between 0.2-1.Omm. The pore sizes of SiO2 / composite scaffolds were mainly distributed in 100-300 渭 m. The pore sizes of gelatin / composite pellet scaffolds were mainly distributed in 100-500 渭 m. The average compressive strength of carboxymethyl cellulose sodium / composite pellet scaffold was about 0.1 MPA, which was mainly distributed in 50-300 渭 m.SiO2 / composite scaffold. The average compressive strength of gelatin / composite microsphere scaffold was 6.3 Mpa.The average compressive strength of carboxymethyl cellulose sodium / composite microsphere biological scaffold was 0.7 Mpa. In vitro biodegradation experiments showed that there was apatite deposition in the process of immersion in SBF of the three scaffolds, which indicated that the scaffolds had good bioactivity. Among them, the degradation cycle of gelatin / composite scaffolds was the longest. The degradation period of carboxymethyl cellulose sodium / composite pellet scaffold was shorter, about 40 days. The biodegradation of SiO2 / composite scaffolds was basically complete on the 80th day of the experiment. The cytotoxicity of the three composite scaffolds was grade 0 or grade 1, that is, no cytotoxicity.
【学位授予单位】：昆明理工大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：TB332;R318.08

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