n-HA/PVA凝胶关节软骨修复材料制备与性能研究
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摘要
聚乙烯醇(PVA)凝胶复合材料是一种潜在的优良关节软骨修复材料。本文采用原位合成和冷冻-解冻相结合的方法制备了纳米羟基磷灰石增强聚乙烯醇(n-HA/PVA)凝胶复合材料。通过多种实验检测手段对凝胶复合材料进行了显微形貌观察和结构表征;系统研究了复合水凝胶材料的力学性能和生物摩擦学性能。主要内容包括:
1.通过在PVA溶液中原位合成n-HA粒子和冷冻-解冻相结合的方法制备n-HA/PVA凝胶复合材料。结果表明,PVA溶液同时起到分散剂的作用,可有效阻止晶粒长大、降低粒子结晶度和提高n-HA的分散性。显微形貌显示随着n-HA含量的增加,复合材料中n-HA粒子趋于团聚。
2.n-HA/PVA凝胶复合材料的应力-应变呈现出典型的非线性特性,是一种粘弹性材料。拉伸和压缩强度均随基体PVA溶液的浓度和冷冻-解冻循环次数的增加而增加,随n-HA含量的增加呈现出先上升后下降的趋势。复合材料的拉伸模量随应变的增加呈线性增加,压缩模量随应变的增加呈指数规律上升。凝胶复合材料的储能模量和损耗模量均随频率、PVA溶液浓度和冷冻-解冻循环次数的增加而增加,随n-HA含量的增加呈现出先上升后下降的变化趋势。当n-HA含量为6%时达最大值。
3.凝胶复合材料的松弛速率随松弛时间的增加而快速下降,随n-HA含量的增加呈现出先上升而后下降的趋势,随初始应变量的增加而增加。归一化平衡松弛模量则随n-HA含量的增加表现为先下降后上升的变化趋势。建立了符合n-HA/PVA凝胶复合材料应力松弛行为的广义Maxwell模型。凝胶复合材料的松弛机理为:凝胶三维网络结构中大量自由水分在短时间内的挤出和聚乙烯醇高聚物键长和键角的瞬时变化导致其快速松弛;网络结构和高分子链段的运动导致中速和慢速松弛。
4.利用Hertz接触理论和弹性流体润滑理论揭示了凝胶复合材料的摩擦系数随不同因素的变化规律。n-HA/PVA凝胶复合材料的摩擦系数随载荷的增加而上升,随摩擦配副不锈钢球半径和滑动速度的增加而下降,随n-HA含量的增加呈现出先下降而后上升的趋势。当n-HA含量为4.5%时,摩擦系数达到最小值0.0458。复合水凝胶在小牛血清润滑条件下的摩擦系数明显低于其在蒸馏水和生理盐水润滑下的摩擦系数。
5.通过改变制备工艺可调控n-HA/PVA凝胶复合材料的力学性能和生物摩擦学性能。较佳制备工艺条件为:复合材料中n-HA含量为6%、基体PVA浓度为20%、冷冻-解冻循环次数为5次。制备的n-HA/PVA复合水凝胶材料具有与自然关节软骨相似结构、力学与摩擦学性能,是一种很有应用前景的关节软骨修复材料。
Poly vinyl alcohol(PVA)hydrogel composite is a promising articular cartilage repairing material.In this dissertation,n-HA/PVA gel composite was prepared by in situ synthesis of nano-HA from PVA solution and combined with freezing/thawing method. The micro-morphology and structure were characterized by many experimental techniques such as TEM,SEM,XRD and FTIR.The mechanical and biotribological properties of n-HA/PVA composite were systemic studied.The main contents and results are as follows:
1.n-HA/PVA gel composite was prepared by in situ synthesis of nano-HA from PVA solution and combined with freezing/thawing method.PVA solution also acted as dispersant to inhibit grain growth,decrease crystallinity degree and improve dispersibility of nano-hydroxyapatite.The results of micro-morphology showed that the nano-hydroxyapatite tents to agglomeration with the increase of nano-hydroxyapatite content in the composite.
2.The change behaviors of tensile and compressive stress of the gel composite with the strain are accorded with non-linear characteristics.Both tensile strength and compressive strength of the composite increase with the rise of PVA solution and freezing/thawing cycle times.The tensile and compressive strength firstly increase and then tend to reducing with the increase of n-HA content.The tensile modulus of the composite increases linearly and compressive modulus increase exponentially with the rise of strain.Both storage and loss modulus of the gel composites increase with test frequency,PVA content and freezing/thawing cycles.The change behavior of their modulus with the rise of HA content represent increase firstly and then decrease.The maximum value of the storage and loss modulus reached while n-HA content in the composites is 6%.
3.The stress relaxation speed of the gel composites decreases rapidly with the rise of relaxation time and increases with the rise of initial strain.At the same initial strain, the stress relaxation speed of the gel composites increases firstly and then tent to decrease.However,the normalized equilibrium relaxation modulus decreases firstly and the increases with the improvement of HA content.The generalized Maxwell model is established to characterize the stress relaxation behavior of the n-HA/PVA gel composites.The stress relaxation mechanism of the composites are:(1)Water rapid extrusion of the composites and the instantaneous change of bond length and bond angle of PVA result in rapid stress relaxation;(2)The movements of network structure and polymeric chain segment cause moderate and slow speed stress relaxations.
4.The change behavior of the gel composites friction coefficient with different influence factors is revealed by Hertz contact theory and elasto-hydrodynamic lubrication theory, The friction coefficient of the gel composites increases with the rise of load and decreases with rise of radium of stainless steel ball and sliding speed.The friction coefficient decreases firstly and then increases with the rise of n-HA content.The minimum value is 0.0458 while n-HA content is 4.5%.The friction coefficient of the gel composites is lower in bovine serum than that in distilled water and physiological saline.
5.The mechanical and bio-triblogical properties of the gel composites can be controlled by varation of processing conditions.For the n-HA/PVA gel composites used as an articular cartilage,the optimum preparation process of n-HA/PVA gel composites is 6wt%HA in 20wt%PVA matrix by 5 freeze/thaw cycle times.n-HA/PVA gel composite is a promising articular cartilage repairing material which possesses similar mechanical and biotribological properties to that of natural articular cartilage.
1.通过在PVA溶液中原位合成n-HA粒子和冷冻-解冻相结合的方法制备n-HA/PVA凝胶复合材料。结果表明,PVA溶液同时起到分散剂的作用,可有效阻止晶粒长大、降低粒子结晶度和提高n-HA的分散性。显微形貌显示随着n-HA含量的增加,复合材料中n-HA粒子趋于团聚。
2.n-HA/PVA凝胶复合材料的应力-应变呈现出典型的非线性特性,是一种粘弹性材料。拉伸和压缩强度均随基体PVA溶液的浓度和冷冻-解冻循环次数的增加而增加,随n-HA含量的增加呈现出先上升后下降的趋势。复合材料的拉伸模量随应变的增加呈线性增加,压缩模量随应变的增加呈指数规律上升。凝胶复合材料的储能模量和损耗模量均随频率、PVA溶液浓度和冷冻-解冻循环次数的增加而增加,随n-HA含量的增加呈现出先上升后下降的变化趋势。当n-HA含量为6%时达最大值。
3.凝胶复合材料的松弛速率随松弛时间的增加而快速下降,随n-HA含量的增加呈现出先上升而后下降的趋势,随初始应变量的增加而增加。归一化平衡松弛模量则随n-HA含量的增加表现为先下降后上升的变化趋势。建立了符合n-HA/PVA凝胶复合材料应力松弛行为的广义Maxwell模型。凝胶复合材料的松弛机理为:凝胶三维网络结构中大量自由水分在短时间内的挤出和聚乙烯醇高聚物键长和键角的瞬时变化导致其快速松弛;网络结构和高分子链段的运动导致中速和慢速松弛。
4.利用Hertz接触理论和弹性流体润滑理论揭示了凝胶复合材料的摩擦系数随不同因素的变化规律。n-HA/PVA凝胶复合材料的摩擦系数随载荷的增加而上升,随摩擦配副不锈钢球半径和滑动速度的增加而下降,随n-HA含量的增加呈现出先下降而后上升的趋势。当n-HA含量为4.5%时,摩擦系数达到最小值0.0458。复合水凝胶在小牛血清润滑条件下的摩擦系数明显低于其在蒸馏水和生理盐水润滑下的摩擦系数。
5.通过改变制备工艺可调控n-HA/PVA凝胶复合材料的力学性能和生物摩擦学性能。较佳制备工艺条件为:复合材料中n-HA含量为6%、基体PVA浓度为20%、冷冻-解冻循环次数为5次。制备的n-HA/PVA复合水凝胶材料具有与自然关节软骨相似结构、力学与摩擦学性能,是一种很有应用前景的关节软骨修复材料。
Poly vinyl alcohol(PVA)hydrogel composite is a promising articular cartilage repairing material.In this dissertation,n-HA/PVA gel composite was prepared by in situ synthesis of nano-HA from PVA solution and combined with freezing/thawing method. The micro-morphology and structure were characterized by many experimental techniques such as TEM,SEM,XRD and FTIR.The mechanical and biotribological properties of n-HA/PVA composite were systemic studied.The main contents and results are as follows:
1.n-HA/PVA gel composite was prepared by in situ synthesis of nano-HA from PVA solution and combined with freezing/thawing method.PVA solution also acted as dispersant to inhibit grain growth,decrease crystallinity degree and improve dispersibility of nano-hydroxyapatite.The results of micro-morphology showed that the nano-hydroxyapatite tents to agglomeration with the increase of nano-hydroxyapatite content in the composite.
2.The change behaviors of tensile and compressive stress of the gel composite with the strain are accorded with non-linear characteristics.Both tensile strength and compressive strength of the composite increase with the rise of PVA solution and freezing/thawing cycle times.The tensile and compressive strength firstly increase and then tend to reducing with the increase of n-HA content.The tensile modulus of the composite increases linearly and compressive modulus increase exponentially with the rise of strain.Both storage and loss modulus of the gel composites increase with test frequency,PVA content and freezing/thawing cycles.The change behavior of their modulus with the rise of HA content represent increase firstly and then decrease.The maximum value of the storage and loss modulus reached while n-HA content in the composites is 6%.
3.The stress relaxation speed of the gel composites decreases rapidly with the rise of relaxation time and increases with the rise of initial strain.At the same initial strain, the stress relaxation speed of the gel composites increases firstly and then tent to decrease.However,the normalized equilibrium relaxation modulus decreases firstly and the increases with the improvement of HA content.The generalized Maxwell model is established to characterize the stress relaxation behavior of the n-HA/PVA gel composites.The stress relaxation mechanism of the composites are:(1)Water rapid extrusion of the composites and the instantaneous change of bond length and bond angle of PVA result in rapid stress relaxation;(2)The movements of network structure and polymeric chain segment cause moderate and slow speed stress relaxations.
4.The change behavior of the gel composites friction coefficient with different influence factors is revealed by Hertz contact theory and elasto-hydrodynamic lubrication theory, The friction coefficient of the gel composites increases with the rise of load and decreases with rise of radium of stainless steel ball and sliding speed.The friction coefficient decreases firstly and then increases with the rise of n-HA content.The minimum value is 0.0458 while n-HA content is 4.5%.The friction coefficient of the gel composites is lower in bovine serum than that in distilled water and physiological saline.
5.The mechanical and bio-triblogical properties of the gel composites can be controlled by varation of processing conditions.For the n-HA/PVA gel composites used as an articular cartilage,the optimum preparation process of n-HA/PVA gel composites is 6wt%HA in 20wt%PVA matrix by 5 freeze/thaw cycle times.n-HA/PVA gel composite is a promising articular cartilage repairing material which possesses similar mechanical and biotribological properties to that of natural articular cartilage.
引文
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