摘要
网化生物陶瓷支架由于良好的三维贯通结构和骨传导性,可以作为细胞粘附、迁移、分化和增殖的三维模板,有利于血管化的形成并引导组织的生长,在组织工程支架领域已经得到非常广泛的应用。但是由于陶瓷的脆性,其力学性能一直无法满足体内承力部位植入的需要,大大限制了它的临床应用。因此,改善网化生物陶瓷支架的力学性能就变得尤为重要。
本文主要采用有机泡沫浸渍法制备网化羟基磷灰石(HA)陶瓷支架,通过比较初始粉体的形状优化制备工艺,然后对网化支架进行力学和生物学性能的优化。分别采用热等静压和聚合物浸涂法改善支架力学性能;同时,为了改善网化支架的生物学性能,利用仿生矿化技术,对网化Ti金属支架、HA/PCL和HA/PDLLA支架进行了表面生物活化,以改善支架对细胞等的亲和性。此外,采用挤压法成功改善了颗粒造孔制备的多孔HA陶瓷支架的贯通性,达到了多孔结构网化目的,同时具有更高的力学性能,并系统考察了造孔颗粒大小等因素对支架力学性能的影响。采用粘度计、体视显微镜、扫描电子显微镜(SEM)、X射线衍射仪(XRD)、和抗压强度测试等分析手段,系统地研究了网化HA支架的性能。获得的主要结论如下:
1.采用有机泡沫浸渍法成功地制备了网化羟基磷灰石(HA)陶瓷支架,研究了不同颗粒形态的HA粉体对网化HA陶瓷支架力学强度的影响,实验结果表明:球形HA粉体所制备的网化陶瓷具有最佳的烧结性能和力学性能,这是由于球形HA粉体颗粒间具有最佳的堆积效果,所配制的浆料具有最高的粘度,因此在样品的浸渍涂覆过程中,泡沫上涂覆的HA浆料最多,因此最终烧结的网化支架的骨架最厚。
2.采用了热等静压、PCL涂层涂覆和PDLLA涂层涂覆等方法改善网化HA陶瓷支架的力学性能,研究了不同方法改善支架力学性能的机理,实验结果表明:1)三种方法均能有效地改善网化HA陶瓷支架的力学性能,采用聚合物涂覆法对支架的力学性能改善更明显;2)热等静压法对支架力学性能的改善是因为在二次烧结过程中,晶粒进一步致密化,使支架内部的微孔和微裂纹明显减少;3)网化HA陶瓷支架涂覆聚己内酯(PCL)和聚乳酸(PDLLA)涂层,不仅在表面能观察到聚合物,在网化多孔结构骨架微孔内部也有一些渗透的聚合物,从而实现了聚合物与陶瓷骨架的复合,在一定程度上降低支架的脆性,达到补强增韧的效果;
3.利用仿生矿化技术对网化支架的多孔结构上进行Ca-P涂层修饰,改善其生物学性能:1)通过在模拟体液(SBF)中仿生矿化,成功地在多孔Ti支架多孔结构表面沉积具有纳米网状结构的Ca-P涂层,支架的三维贯通结构不变;2)通过在过饱和的钙磷溶液(SCPS)中仿生矿化,成功在HA/PCL复合支架表面修饰具有片层状结构的Ca-P涂层;3)在PDLLA涂层中添加CaSO_4和硫酸软骨素(CS)颗粒可以成功地改善复合支架的生物活性,在SBF中仿生矿化7天和14天后支架表面出现纳米网状结构的Ca-P涂层,添加CaSO_4的复合支架的生物活性更好;SBF的浓度会影响仿生矿化Ca-P涂层的微观结构,在1倍SBF中Ca-P涂层呈纳米网状结构,在1.5倍SBF中呈片层状结构。
4.采用挤压法成功地改善颗粒造孔工艺制备的多孔HA陶瓷支架的贯通性,实现了完全网化的多孔贯通结构;造孔剂的颗粒大小基本不影响支架的孔隙率;支架的收缩率与造孔剂蜡球大小和成形剂甲壳素无关;影响支架收缩率的主要因素是HA的浓度,HA的浓度越高,支架的收缩率越小,但过高的HA浓度不利于支架的收缩;造孔剂粒度对支架的抗压强度有明显影响:随着蜡球粒度的增大,对应的网化HA陶瓷支架的抗压强度逐渐降低。
Porous hydroxyapatite (HA) ceramic scaffolds are universally used for bone repair and replacement, and for serving functions to support the adhesion, transfer, proliferation and differentiation of cells due to the three-dimensional (3D) interconnected structure. Due to the brittleness of HA bioceramics, these scaffolds are not suitable to clinical load-bearing sites with the poor strength. Therefore, the application of porous HA bioceramics have been restricted. It is significant to improve the mechanical properties of porous HA bioceramics while maintained the high porosity.
The polymer impregnating method was firstly adopted to produce porous hydroxyapatite (HA) ceramic scaffolds with 3D porous structures. The preparation process of porous HA bioceramics are optimized by investigating the concentrations of HA slurry, coating times and particle morphologies. Then, the Hot Isostatic Pressing (HIP) and polymer-coating methods were used to enhance the mechanical strength of porous HA bioceramics. At the same time, considering the biological properties, biomineralization technique was employed for porous Titanium (Ti), HA/PCL and HA/PDLLA scaffolds to improve the affinity to cell. The effect of some bioactive phases including HA, CaSO_4 and CS are investigated by introducing into the polymer coating. Besides, the interconnectivity of porous HA bioceramics fabricated by particle leaching are successfully improved by using extrusion method. The results show that the prepared HA bioceramics scaffolds possess excellent foam-like structure and mechanical properties. Nanoindenter, rotating viscosimeter, stereomicroscope, scanning electron microscopy (SEM), X-ray diffractometer (XRD) and mechancail tester were used to study the properties of porous HA bioceramics scaffold. Main conclusions are drawn as follows:
1. The porous HA scaffold with highly porous structure are successfully prepared by polymer impregnating method. The influence of particle morphologies on mechanical strength of porous HA bioceramics scaffold were investigated. The results showed that the porous HA bioceramics made from spherical HA particles held a higher compressive strength and sintering properties than when using other HA particles morphologies. The use of spherical particles in the preparation process of porous HA bioceramics proved to form the most homogeneous slurry with a higher viscosity, and held more coating on the PU template for the same impregnating process.
2. HIP, PCL-coating and PDLLA-coating methods were used to enhance the mechanical properties of porous HA bioceramics scaffold. The strength mechanism of different methods was studies in detail. The results showed that: 1) All three methods are useful to enhance the mechanical properties of porous HA bioceramics, which is better by using the polymer-coating method. 2) As a technique to enhance the sintering and densification of ceramics, the HIP treatment is effective to improve the mergence between grains during the sintering process. Micropores and microcracks decrease significantly in struts of HIP-treated HA scaffolds. 3) PCL lining and PDLLA lining can serve to protect and support the scaffold in the initial stage of use after its implantation in vivo under different load bearing conditions, while the intergranular polymer can strengthen the bridge connection between the particles to prevent the crack propagation or the alteration of its pathway.
3. The biomimetic mineralization technique was employed to modify the biological properties of porous structure by depositing Ca-P coating. 1) The nano net-like structure of Ca-P was deposited on the porous Ti scaffold by immersed in simulated body fluid (SBF) and had no influence on the interconnectivity of Ti scaffold. 2) The plate-like Ca-P was successfully deposited on the HA/PCL composite scaffold by immersed in supersaturation calcium phosphate solution (SCPS). 3) The introduction of bioactive phase (HA、CaSO_4 and CS) into PDLLA coating effectively enhanced the bioactivity of composite scaffold. After 7 and 14 days immersion in SBF, a nano net-like Ca-P coating were found on the surface of composite scaffolds. The bioactivity of the composite scaffolds with CaSO_4 is higher than the other composite scaffolds. With the increase of the concentration of SBF, the morphologies of deposited apatite are plate-like different from the net-like apatite immersed in 1SBF.
4. Extrusion method is significant to improve the interconnectivity of porous HA bioceramics scaffold prepared by particle leaching method that hold excellent mechanical properties. The size of pore former of wax has no influence on the porosity (about 86%) of porous HA bioceramics. The shrinkage ratio (56%) of the three sinter porous HA bioceramics scaffolds have nothing to do with the particle size and chitin formagen except the HA concentration. With the increase of HA concentration, the shrinkage ratio of scaffold is descendent. The particle size have obvious effect on the compressive strength: with the increase of the size of wax, the compressive strength of porous HA bioceramics scaffold present a gradual decreasing tendency.
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