挤出法制备多孔磷酸钙骨修复材料
发布时间：2018-12-18 21:51
【摘要】：本论文针对目前制备多孔磷酸钙骨修复材料在成型方法和性能上存在的不足,首次采用挤出成型法,利用自合成β-磷酸三钙(β-TCP)粉体制备了蜂窝状多孔β-TCP骨修复材料。通过添加造孔剂对挤出制备的多孔材料的孔壁进行了造孔,形成出具有宏孔(挤出成型孔)、微米孔(排除造孔剂颗粒形成的孔)和亚微米孔(烧结孔)的三级孔磷酸钙陶瓷骨修复材料,并通过在β-TCP合成过程中同步引入焦磷酸钙改善多孔β-TCP陶瓷的强度,通过灌注技术调节挤出宏孔的尺寸和形状,制备出了同时具有高孔隙率、单向连通、孔径可控、孔径均匀、抗压强度较高的多级孔磷酸钙骨修复材料。 首先,设计了合适的挤出成型模具,采用活塞式液压挤出成型方法,制备具有孔径可调、孔径均匀、开口孔率高、力学性能好、适合工业化生产等优点的多孔支架。采用湿式粉碎法合成β-TCP、CPP/β-TCP粉体,研究了β-TCP和CPP/β-TCP粉体的可成型性。实验表明:所合成的β-TCP和CPP/β-TCP粉体都适用于采用挤出成型。将粉体和各添加剂按照一定的顺序进行混炼,得到可塑性好的泥团。采用正交试验法,得出了在β-TCP粉体成型过程中各添加剂的最佳配比为甲基纤维素M450 8%、液体石蜡10 %和去离子水32 %。并对影响挤出多孔材料结构和性能的因素,包括挤出压力、干燥制度、烧成制度、模具结构等进行了实验分析,通过实验确定了较合理的工艺参数。所制备的蜂窝状多孔β-TCP骨修复材料具有较理想的结构和性能。挤出成型的多孔材料,挤出孔呈方形,孔径基本一致,约为850μm,孔隙率约为74 %,抗压强度约为17 MPa。 为了进一步提高蜂窝状多孔β-TCP材料孔壁的孔隙率,本研究通过添加马铃薯淀粉作为造孔剂对孔壁进行了造孔。实验结果表明:当造孔剂在生坯中分布较均匀时,在蜂窝状多孔材料孔壁中所形成孔隙的孔径分布也较均匀;当马铃薯淀粉添加量为30%时,材料的总孔隙率提高到85 %,此时抗压强度降低到约4.5 MPa,仍可基本满足作为组织工程支架或非负重部位骨缺损修复材料的要求。为提高蜂窝状多孔β-TCP材料的力学性能,本实验通过改变原料的化学计量数之比,同步合成了不同焦磷酸钙(CPP)含量的CPP/β-TCP混合粉,研究了引入CPP对多孔β-TCP陶瓷的结构和性能的影响。实验表明,CPP的引入通过在高温下与β-TCP形成共融物促进烧结,并稳定β-TCP晶相,从而可以提高β-TCP的烧结温度,获得更高材料烧结致密度,使多孔β-TCP陶瓷的抗压强度得到提高。在造孔剂添加量为30 %的情况下,当CPP含量为5 %,采用在1200℃保温1 h的烧成制度,CPP/β-TCP多孔生物陶瓷的抗压强度提高到约6.5 MPa。 本论文对比研究了几种多孔磷酸钙陶瓷材料的降解性能。研究表明,未加造孔剂制备的β-TCP多孔材料在PBS溶液中浸泡的过程是溶解与重结晶共同发生的过程,在材料表面析出针状晶体,但加入了造孔剂制备的β-TCP和5%CPP/β-TCP多孔材料在PBS溶液中没有发生明显的析晶。添加30 %造孔剂进行孔壁造孔的多孔材料在PBS溶液中随着浸泡时间的延长失重率有所增大,其中多孔5%CPP/β-TCP陶瓷的降解速率高于多孔β-TCP陶瓷。 另外,对于“适于骨组织长入的孔径”这一问题,学者们所持观点不一。本研究采用灌浆法调节蜂窝状多孔材料的孔道尺寸、孔形状,可以根据需要减小孔径,通过灌注使孔道的直角变成圆弧角,有利于细胞的爬移。而且通过灌浆,提高了多孔磷酸钙材料的力学性能。 细胞实验表明,所制备的多孔磷酸钙材料具有良好的生物相容性,细胞在材料表面铺展良好,且细胞在材料中可维持较好的增殖能力。
[Abstract]:In this paper, for the defects of the present preparation method and properties of the porous calcium phosphate bone repair material, the honeycomb-shaped porous calcium phosphate-TCP bone repair material was prepared by using the self-synthetic calcium-phosphate tricalcium (HCO3-TCP) powder for the first time. the hole wall of the porous material prepared by extrusion is made through the addition of a pore-making agent to form a three-stage hole calcium phosphate ceramic bone repairing material with a macro hole (extrusion forming hole), a micro-hole (hole for removing the pore-forming agent particle) and a sub-micron hole (sintering hole), and the strength of the porous carbon-TCP ceramic is improved by synchronously introducing the calcium pyrophosphate in the TCP-TCP synthesis process, the size and the shape of the extruded macro hole are adjusted through the perfusion technology, the high porosity, the one-way communication is prepared, the aperture is controllable, the aperture is uniform, a multi-stage pore calcium phosphate bone repair material with higher compressive strength. firstly, a suitable extrusion molding die is designed, and a piston type hydraulic extrusion molding method is adopted to prepare a porous branch with the advantages of adjustable aperture, uniform aperture, high aperture ratio, good mechanical property, suitability for industrial production and the like. The formation of TCP, CPP and CP-TCP powders by wet-milling is used to study the formation of TCP and CPP/ CP-TCP powders. The experimental results show that the synthesized TCP-TCP and CPP/ CP-TCP powders are suitable for extrusion. The method comprises the following steps of: mixing the powder and the additives according to a certain sequence to obtain the mud with good plasticity The optimum proportion of each additive is methyl cellulose M450 8%, liquid paraffin 10% and deionized water 32. The factors that affect the structure and properties of the extruded porous material, including the extrusion pressure, the drying system, the firing system, the mould structure and so on, are analyzed, and the reasonable process parameters are determined by the experiment. and the prepared honeycomb-shaped porous polystyrene-TCP bone repairing material has the ideal structure and the property, The extrusion-molded porous material, the extrusion orifice is square, the aperture is substantially uniform, about 850. m u.m, the porosity is about 74%, the compressive strength is about 17MP, a. In order to further improve the porosity of the cellular porous carbon-TCP material hole wall, the present study was conducted by adding potato starch as a pore-making agent to the hole wall. The experimental results show that when the pore-forming agent is distributed more uniformly in the green body, the pore size distribution of the pore formed in the hole wall of the cellular porous material is also uniform; when the amount of the potato starch is 30%, the total porosity of the material is increased to 85%, and the compressive strength is reduced to about 4.5. MPa, and can still be basically satisfied as a tissue engineering scaffold or a non-weight-bearing part bone defect repairing material In order to improve the mechanical properties of the cellular porous TCP/ TCP material, the CPP/ I-TCP mixed powder with different content of calcium pyrophosphate (CPP) was synthesized by changing the ratio of the stoichiometric ratio of the raw materials, and the structure and properties of the introduced CPP to the porous PTFE-TCP ceramics were studied. The experiment shows that the introduction of CPP promotes the sintering by the formation of a blend with the C-TCP at high temperature, and stabilizes the sintered-TCP phase, so that the sintering temperature of the P-TCP can be improved, the density of the higher material sintering can be obtained, and the compressive strength of the porous sintered-TCP ceramic can be obtained. When the addition amount of the pore-making agent is 30%, when the content of the CPP is 5%, the compression strength of the CPP/ L-TCP porous bioceramics is increased to about 6.5 when the content of the CPP is 5%, the firing system with the temperature of 1200 DEG C for 1h is adopted, and the compressive strength of the CPP/ L-TCP porous bioceramics is improved to about 6.5. In this paper, several kinds of porous calcium phosphate ceramic materials are studied in this paper. The results of the study show that the process of soaking the porous-TCP porous material in the solution of PBS is the process of co-occurrence of the dissolution and recrystallization in the solution of PBS, and the surface of the material The needle-like crystals were out, but the P-TCP and 5% CPP/ I-TCP porous materials prepared with the pore-making agent did not occur in the PBS solution and the degradation rate of the porous 5% CPP/ L-TCP ceramic is higher than that of the porous material-TCP ceramics. In addition, for 鈥減ore size suitable for bone tissue growth鈥，
本文编号：2386548
[Abstract]:In this paper, for the defects of the present preparation method and properties of the porous calcium phosphate bone repair material, the honeycomb-shaped porous calcium phosphate-TCP bone repair material was prepared by using the self-synthetic calcium-phosphate tricalcium (HCO3-TCP) powder for the first time. the hole wall of the porous material prepared by extrusion is made through the addition of a pore-making agent to form a three-stage hole calcium phosphate ceramic bone repairing material with a macro hole (extrusion forming hole), a micro-hole (hole for removing the pore-forming agent particle) and a sub-micron hole (sintering hole), and the strength of the porous carbon-TCP ceramic is improved by synchronously introducing the calcium pyrophosphate in the TCP-TCP synthesis process, the size and the shape of the extruded macro hole are adjusted through the perfusion technology, the high porosity, the one-way communication is prepared, the aperture is controllable, the aperture is uniform, a multi-stage pore calcium phosphate bone repair material with higher compressive strength. firstly, a suitable extrusion molding die is designed, and a piston type hydraulic extrusion molding method is adopted to prepare a porous branch with the advantages of adjustable aperture, uniform aperture, high aperture ratio, good mechanical property, suitability for industrial production and the like. The formation of TCP, CPP and CP-TCP powders by wet-milling is used to study the formation of TCP and CPP/ CP-TCP powders. The experimental results show that the synthesized TCP-TCP and CPP/ CP-TCP powders are suitable for extrusion. The method comprises the following steps of: mixing the powder and the additives according to a certain sequence to obtain the mud with good plasticity The optimum proportion of each additive is methyl cellulose M450 8%, liquid paraffin 10% and deionized water 32. The factors that affect the structure and properties of the extruded porous material, including the extrusion pressure, the drying system, the firing system, the mould structure and so on, are analyzed, and the reasonable process parameters are determined by the experiment. and the prepared honeycomb-shaped porous polystyrene-TCP bone repairing material has the ideal structure and the property, The extrusion-molded porous material, the extrusion orifice is square, the aperture is substantially uniform, about 850. m u.m, the porosity is about 74%, the compressive strength is about 17MP, a. In order to further improve the porosity of the cellular porous carbon-TCP material hole wall, the present study was conducted by adding potato starch as a pore-making agent to the hole wall. The experimental results show that when the pore-forming agent is distributed more uniformly in the green body, the pore size distribution of the pore formed in the hole wall of the cellular porous material is also uniform; when the amount of the potato starch is 30%, the total porosity of the material is increased to 85%, and the compressive strength is reduced to about 4.5. MPa, and can still be basically satisfied as a tissue engineering scaffold or a non-weight-bearing part bone defect repairing material In order to improve the mechanical properties of the cellular porous TCP/ TCP material, the CPP/ I-TCP mixed powder with different content of calcium pyrophosphate (CPP) was synthesized by changing the ratio of the stoichiometric ratio of the raw materials, and the structure and properties of the introduced CPP to the porous PTFE-TCP ceramics were studied. The experiment shows that the introduction of CPP promotes the sintering by the formation of a blend with the C-TCP at high temperature, and stabilizes the sintered-TCP phase, so that the sintering temperature of the P-TCP can be improved, the density of the higher material sintering can be obtained, and the compressive strength of the porous sintered-TCP ceramic can be obtained. When the addition amount of the pore-making agent is 30%, when the content of the CPP is 5%, the compression strength of the CPP/ L-TCP porous bioceramics is increased to about 6.5 when the content of the CPP is 5%, the firing system with the temperature of 1200 DEG C for 1h is adopted, and the compressive strength of the CPP/ L-TCP porous bioceramics is improved to about 6.5. In this paper, several kinds of porous calcium phosphate ceramic materials are studied in this paper. The results of the study show that the process of soaking the porous-TCP porous material in the solution of PBS is the process of co-occurrence of the dissolution and recrystallization in the solution of PBS, and the surface of the material The needle-like crystals were out, but the P-TCP and 5% CPP/ I-TCP porous materials prepared with the pore-making agent did not occur in the PBS solution and the degradation rate of the porous 5% CPP/ L-TCP ceramic is higher than that of the porous material-TCP ceramics. In addition, for 鈥減ore size suitable for bone tissue growth鈥，
本文编号：2386548
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