HA/316L不锈钢生物功能梯度材料研究
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摘要
羟基磷灰石(HA)具有优良的生物相容性,作为人工骨已广泛应用于骨缺损的修复,但其力学性能较差,限制了其作为承重骨的使用;而临床上普遍应用的力学性能优越的金属植入体316L不锈钢(以下简称316L)因其生物相容性较差而导致炎症等不良反应。制备兼具二者性能优点的复合材料已成为当今生物材料领域的研究热点之一。本论文围绕这一重要课题,采用粉末冶金法制备了HA/316L生物复合材料;并针对HA/316L两相热应力不匹配的问题,制备了热应力缓和的HA/316L生物功能梯度材料(FGM),对其力学性能、物相组成、显微结构以及生物相容性评价进行了较系统深入的研究。
首先制备了HA和ZrO_2(CaO)纳米粉末。结果表明:随着HA前驱体煅烧温度的逐渐升高,HA晶化程度越来越高,其最佳制备工艺为以5℃·min~(-1)升温速率升至750℃后保温2h。通过对HA晶粒尺寸和煅烧温度的相关计算求得HA的生长活化能为24.8kJ·mol~(-1),并提出HA晶粒长大主要为界面扩散控制机制。采用化学共沉淀与共沸蒸馏相结合在600℃至1100℃温度范围内热处理后可得到掺杂5mol%CaO的四方相ZrO_2(CaO)纳米粉末,该纳米粉末由四方相向单斜相转变的临界温度为1234.5℃,高于纯氧化锆纳米粉的转变温度,初步推断是由于稳定剂氧化钙的存在所致。
通过真空烧结制备了HA/316L粉、HA/316L纤维和HA-ZrO_2(CaO)/316L纤维系列生物复合材料,综合力学性能顺序为HA/316L粉系 首次研究了316L纤维的长度、直径与含量对HA-ZrO_2(CaO)/316L纤维生物复合材料的力学性能的影响规律。结果表明:纤维直径为40μm的复合材料力学性能优于纤维直径为50μm的复合材料;纤维长度为0.8～1.2mm的复合材料力学性能优于纤维长度为2～3mm的复合材料;随着纤维体积分数增大,纤维之间相互接触而导致在复合材料中形成的微孔增多,并成为微裂纹源,导致材料力学性能下降。含20vol%直径为40μm、长度为0.8～1.2mm的316L纤维的
Hydroxyapatite(HA) has excellent biocompatibility and bad mechanical properties, which restricts its usage for bearing bone reconstruction. 316L stainless steel(316L) has broad applications in clinic, but it always lead to ill reaction such as inflammation because of its unqualified biocompatibility. Preparation of the composites having both advantages has become the heat point in biomaterials field. Surrounding this important task, HA/316L biocomposites were fabricated with powder metallurgy in this paper. Aim at the question of heat stress mismatch between HA and 316L phase, heat stress relaxed HA/316L biological functionally gradient materials(FGM) were prepared. At the same time, systemic researches including mechanical properties, phase structure, microstructure and biocompatibility evaluation of the FGM were carried out.HA and ZrO_2 ( CaO ) nano powder were prepared firstly. The results show that crystal degree of hydroxyapatite enhance with the increase of calcinated temperature and the optimal preparing technique is maintaining 2h at 750℃ with temperature-rising speed of 5℃·min~-1. Activated energy of HA can be calculated as 24.8 kJ·mol~-1 according to the relationship between grain size and calcinated temperature. HA's growing mechanism is interficial diffusion controlling mechanism. ZrO_2 ( CaO ) nano powder is prepared by azeotropic distillation and chemical coprecipitation method with heat treatment between 600 ℃ and 1 100 ℃ . Transformation temperature of tetragonal phase to monoclinic phase is 1 234.5 ℃ in ZrO_2 ( CaO ) nano powder, which is higher than that of pure ZrO_2 because of the existence of stabilizer CaO.HA/316L power, HA/316L fibre and HA-ZrO_2 (CaO) /316L fibre biocomposite series were fabricated by vacuum sintering. The results show that comprehensive mechanical properties can be ranked as HA/316L power system system. Microstructure of all biocomposite systems change regularly with the components of HA and interface of HA/316L powder(or HA/316L fibre) combines tightly. Some element interdiffusion takes place between both phases in HA/316L power system and Ca, P element' s diffusibility in HA is laeger than that of Fe element in 316L powder. While there only exists diffusion of Fe element in 316L fibre to the matrix in HA/316L fibre and HA-ZrO2 (CaO) /316L systems.The approaches also address that diameter and length of 316L fibre have influence to the mechanical properties of HA-ZrO2 (CaO) /316L biocomposites. Composite's mechanical properties with fibre diameter of 40 u m is better than that of 50 U m and fibre length of 0.8-1.2mm is better that of 2~3mm. Micropores increase with volume fraction of 316L fibre because of contact among fibres, which become microflaws and lead to descending of mechanical properties. Thereof, it can be concluded that HA-ZrO2 (CaO) /316L fibre biocomposite having 20vol% with fibre diameter of 40 u m and fibre length of 0.8~1.2mm has optimal mechanical properties with bending strength, Young's modulus and fracture toughness equal tol40.1MPa, 117.8GPa and 5.81 MPa-m m, 87.1%, respectively.HA-ZrO2 (CaO) /316L fibre symmetrical and asymmetrical biological FGMs were fabricated under 1100°C by use of hot isostatic pressing(HIP) technique. The results show that there is no distortion in the FGMs and no microcracks on their surface. 316L fibre is evenly distributed in the FGMs. 316L fibre is enwrapped in the HA-ZrO2 ( CaO ) matrix and both integrate each other tightly. The combining mechanism of matrix to 316L fibre is physical adhering force. With increase of HA contents, both fracture toughness and Young's modulus of the gradient layer in HA-ZrO2 (CaO) /316L fibre FGMs decrease gradually, which results in mechanical properties relaxation design of the FGMs. It can be deduced that fibre pulling out and interbedded crack deflexion are the major toughing mechanism in the FGMs.HA/316L powder symmetrical and asymmetrical FGMs were
fabricated by hot pressing(HP) technique. The results show that obvious gradient changes on the macroscopic are shown in the FGMs. While the components changes continuously in microcosmic and the interfaces among all gradient layers unites tightly. The addition of 316L powder changes the fracture way of the composites and improves their mechanical properties. There exists several toughing mechanism including interbedded crack deflexion, crack deflexion and crack bridging in the FGMs.HA contents in HA/316L biological FGMs change regularly with different gradient layer, which is coincided with the componets design. Grain size of 316L grows gradually with the decrease of HA contents, which suggests HA has restraining erTect on the growth of 316L grain size. Major sub-structure of 316L component are dislocation and stacking. Conbining circumstance of phase interface is very well and both phase bite into each other at the interface. There approximately exists 20 nm transition area at the interface. The two phases of HA and 316L powder dissolve into each other in some degree during hot pressing and the combining mechanism is dissolving behavior.Acute toxicity experiment, sub-acute toxicity experiment, heat resource experiment, bacteria-restraining experiment, blood-dissolving experiment, skin-implanting experiment, Ames experiment and cell toxicity experiment were carried out to HA/316L powder FGMs. The results show that HA/316L powder FGMs have excellent biocompatibility and possess broad clinical value in bearing bone reconstruction.
首先制备了HA和ZrO_2(CaO)纳米粉末。结果表明:随着HA前驱体煅烧温度的逐渐升高,HA晶化程度越来越高,其最佳制备工艺为以5℃·min~(-1)升温速率升至750℃后保温2h。通过对HA晶粒尺寸和煅烧温度的相关计算求得HA的生长活化能为24.8kJ·mol~(-1),并提出HA晶粒长大主要为界面扩散控制机制。采用化学共沉淀与共沸蒸馏相结合在600℃至1100℃温度范围内热处理后可得到掺杂5mol%CaO的四方相ZrO_2(CaO)纳米粉末,该纳米粉末由四方相向单斜相转变的临界温度为1234.5℃,高于纯氧化锆纳米粉的转变温度,初步推断是由于稳定剂氧化钙的存在所致。
通过真空烧结制备了HA/316L粉、HA/316L纤维和HA-ZrO_2(CaO)/316L纤维系列生物复合材料,综合力学性能顺序为HA/316L粉系
Hydroxyapatite(HA) has excellent biocompatibility and bad mechanical properties, which restricts its usage for bearing bone reconstruction. 316L stainless steel(316L) has broad applications in clinic, but it always lead to ill reaction such as inflammation because of its unqualified biocompatibility. Preparation of the composites having both advantages has become the heat point in biomaterials field. Surrounding this important task, HA/316L biocomposites were fabricated with powder metallurgy in this paper. Aim at the question of heat stress mismatch between HA and 316L phase, heat stress relaxed HA/316L biological functionally gradient materials(FGM) were prepared. At the same time, systemic researches including mechanical properties, phase structure, microstructure and biocompatibility evaluation of the FGM were carried out.HA and ZrO_2 ( CaO ) nano powder were prepared firstly. The results show that crystal degree of hydroxyapatite enhance with the increase of calcinated temperature and the optimal preparing technique is maintaining 2h at 750℃ with temperature-rising speed of 5℃·min~-1. Activated energy of HA can be calculated as 24.8 kJ·mol~-1 according to the relationship between grain size and calcinated temperature. HA's growing mechanism is interficial diffusion controlling mechanism. ZrO_2 ( CaO ) nano powder is prepared by azeotropic distillation and chemical coprecipitation method with heat treatment between 600 ℃ and 1 100 ℃ . Transformation temperature of tetragonal phase to monoclinic phase is 1 234.5 ℃ in ZrO_2 ( CaO ) nano powder, which is higher than that of pure ZrO_2 because of the existence of stabilizer CaO.HA/316L power, HA/316L fibre and HA-ZrO_2 (CaO) /316L fibre biocomposite series were fabricated by vacuum sintering. The results show that comprehensive mechanical properties can be ranked as HA/316L power system
fabricated by hot pressing(HP) technique. The results show that obvious gradient changes on the macroscopic are shown in the FGMs. While the components changes continuously in microcosmic and the interfaces among all gradient layers unites tightly. The addition of 316L powder changes the fracture way of the composites and improves their mechanical properties. There exists several toughing mechanism including interbedded crack deflexion, crack deflexion and crack bridging in the FGMs.HA contents in HA/316L biological FGMs change regularly with different gradient layer, which is coincided with the componets design. Grain size of 316L grows gradually with the decrease of HA contents, which suggests HA has restraining erTect on the growth of 316L grain size. Major sub-structure of 316L component are dislocation and stacking. Conbining circumstance of phase interface is very well and both phase bite into each other at the interface. There approximately exists 20 nm transition area at the interface. The two phases of HA and 316L powder dissolve into each other in some degree during hot pressing and the combining mechanism is dissolving behavior.Acute toxicity experiment, sub-acute toxicity experiment, heat resource experiment, bacteria-restraining experiment, blood-dissolving experiment, skin-implanting experiment, Ames experiment and cell toxicity experiment were carried out to HA/316L powder FGMs. The results show that HA/316L powder FGMs have excellent biocompatibility and possess broad clinical value in bearing bone reconstruction.
引文
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