纳米磷酸钙、硅酸钙及其复合生物与环境材料的制备和性能研究
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摘要
本论文在制备磷酸钙(β-Ca_3(PO_4)_2,β-TCP;Ca_(10)(PO_4)_6(OH)_2,HAp)纳米粉体、水合硅酸钙(Ca_5Si_6O_(16)(OH)_2·4H_2O,Tobermorite;Ca_6Si_6O_(17)(OH)_2,Xonotlite)纳米线、硅酸钙(CaSiO_3,CS)超细粉体和纳米线、β-TCP/CS和HAp/CS纳米复合粉体的基础上,研究了水合硅酸钙Tobermorite纳米线的体外生物活性和降解性;研究了磷酸钙和硅酸钙纳米粉体的烧结性能和烧结体的相关性能;研究了β-TCP/CS和HAp/CS纳米复合生物陶瓷的制备及复合比例对材料的力学性能、生物活性和降解性的影响规律;探索了高强度大孔β-TCP和CS陶瓷支架材料的制备技术、具有天然松质骨结构的β-TCP和CS陶瓷支架材料的制备技术,并研究了多孔支架材料的生物相容性、生物活性、降解性和骨修复性能;最后还探索了HAp对水溶液中酚类化合物吸附性能。具体研究内容和结果如下:
1、(1)应用化学沉淀法、水热微乳液法、超声化学法和水热均相沉淀法,并通过控制工艺条件可以制备得到不同形貌、结晶度、颗粒尺寸和比表面积的HAp纳米粉体;(2)采用化学沉淀法可以规模化制备得到颗粒尺寸约80～100nm的β-TCP纳米粉体;(3)采用水热微乳液法制备得到分散性良好的、颗粒细小且晶粒尺寸分布窄的Tobermorite纳米线,纳米线的直径约30～50nm,长度最高达10多微米;(4)采用简单的水热处理法制备了分散性良好的Xonotlite纳米线,粉体直径约10～30nm、长度可以达10多微米,Xonotlite纳米线于800℃煅烧2h获得CS纳米线,粉体的形貌和尺寸基本保持不变;(5)采用两步化学沉淀法制备得到复合比例可控的、分散性良好的β-TCP/CS和HAp/CS纳米复合粉体,粉体颗粒尺寸分别为20～80nm和10～30nm。
2、研究了Tobermorite纳米线的体外生物活性和降解性。研究表明Tobermorite纳米线在模拟体液(Simulated body fluid,SBF)中具有良好的生物活性(诱导沉积类骨HAp的能力)和降解性。在SBF中浸泡3d,表面即完全被类骨HAp覆盖;14d的降解率达24.5wt.%。Tobermorite纳米线降解后溶液介质的pH明显升高,该性能使其可被应用于中和聚酯类生物高分子的酸性降解产物,以避免这类传统高分子材料因降解产生的酸性产物而引发的无菌性炎症反应。研究结果显示Tobermorite纳米线有望作为良好的可降解生物活性增强体应用于制备生物活性复合材料。
3、以纳米粉体为原料,采用干压、冷等静压成型技术,通过控制烧结工艺制备了磷酸钙和硅酸钙生物陶瓷材料。研究表明纳米粉体具有良好的烧结活性,并可以制备得到晶粒细小的、高致密度的烧结体,从而获得力学性能良好的磷酸钙和硅酸钙生物陶瓷材料:(1)采用常规无压烧结工艺制备了高强度的β-TCP生物陶瓷,其抗弯强度高达200MPa,是微米粉体烧结体的2倍,且明显高于文献报道的结果。(2)采用放电等离子体烧结工艺(Spark PlasmaSintering,SPS)制备得到透明β-TCP生物陶瓷,平均晶粒尺寸约250 nm,具有良好的透光性能、最大透光率约52%(1mm厚)。细胞相容性研究结果表明,透明β-TCP生物陶瓷对骨髓间质干细胞的增殖作用明显高于常规的通用聚乙烯培养板,可望作为新型的细胞培养载体材料和医学窗口材料。(3)常压下,采用简单的两步烧结工艺(Two-step Sintering Method,TSM)制备得到平均晶粒尺寸为193nm的致密HAp纳米生物陶瓷材料,其晶粒尺寸明显低于传统的无压烧结工艺(高达765nm),TSM制备得到的HAp纳米生物陶瓷材料的韧性达1.18MPa·m~(1/2),较无压烧结工艺提高了约60%。(4)采用CS纳米线于1100℃无压烧结3h可以获得抗弯强度约146MPa、与人体皮质骨强度的上限值相当,其强度较CS超细粉体烧结体提高了约53%,而弹性模量也与人体致密骨相当。研究结果表明采用纳米线有望获得力学强度较好的CS生物陶瓷材料。(5)CS生物陶瓷具有良好的生物活性、降解性和细胞相容性,在SBF中浸泡1d后即可在表面沉积一层类骨HAp层,表明材料具有良好的生物活性,在Tris-HCl缓冲液浸泡28d的降解率达27.85%、远高于β-TCP的降解率(仅2.51%),骨髓间质干细胞的贴壁和增殖实验表明CS陶瓷具有良好的生物相容性。研究结果表明CS生物陶瓷材料有望作为新型的可降解生物活性骨修复材料。
4、以纳米复合粉体为原料,采用干压、冷等静压成型技术,并采用无压烧结工艺制备了β-TCP/CS纳米复合生物陶瓷材料。研究表明复合生物陶瓷的力学性能、生物活性和降解性可以通过复合比例加以有效调控。当β-TCP的复合比例高于50wt.%时,即可制备得到力学强度与人体皮质骨相当的复合生物陶瓷材料,且强度随β-TCP复合比例的提高明显升高;而当CS的复合比例超过30wt.%时,材料即显示优越的生物活性,在SBF中浸泡1d即完全被类骨HAp层覆盖,且复合陶瓷的生物活性和降解性随CS组分的含量增加而提高。
5、以纳米复合粉体为原料,采用干压、冷等静压成型技术,并采用无压烧结工艺制备了CS/HAp纳米复合生物陶瓷材料。研究表明复合生物陶瓷的力学性能、生物活性和降解性可以通过复合比例加以有效调控。通过调节复合比例,CS/HAp复合陶瓷的抗弯强度可以控制在98.06～221.30MPa,当CS复合比例高于50wt.%时,材料的强度显著高于人体皮质骨,而弹性模量与人体致密骨相当。复合陶瓷的生物活性和降解性随CS组分含量的提高而增强。
6、采用添加造孔剂法、注浆成型工艺和泡沫浸渍工艺制备了多孔β-TCP和CS生物陶瓷支架材料。实验表明采用添加造孔剂法和注浆成型工艺制备得到的材料力学强度较好,采用注浆成型工艺和泡沫浸渍工艺可以获得孔连通性良好的多孔陶瓷支架材料,而采用泡沫浸渍工艺还可以获得与天然松质骨结构相类似的多孔陶瓷支架材料。同时,采用纳米粉体可以制备得到力学强度良好的β-TCP多孔陶瓷支架材料。SBF浸泡实验表明,CS支架在SBF中浸泡1d表面就全部被类骨HAp层覆盖住,同时支架材料具有良好的降解性,气孔率为63.1%的支架材料7d的降解率达7.14%。研究结果表明多孔CS生物陶瓷支架材料有望作为新型的可降解生物活性骨修复材料和骨组织工程支架材料。
7、研究了多孔β-CS和CS生物陶瓷支架材料的非骨性环境下的生物学行为、以及兔子颅骨的缺损修复性能。研究表明,多孔CS生物陶瓷在早期血管化、新生组织长入、材料降解性和骨修复能力等方面均较传统的β-TCP生物陶瓷具有明显优势。动物植入实验还表明细胞调节作用参与了CS材料的体内降解过程;SEM和EDS分析结果表明新生骨生成于CS材料诱导沉积的类骨HAp层表面,而不是直接作用于CS材料表面,表明生成的类骨HAp层对新骨的生成、以及材料同骨组织的键合作用起关键作用。动物植入试验研究结果表明,多孔CS陶瓷材料有望作为可降解生物活性材料应用于硬组织修复和骨组织工程材料领域。
8、以HAp纳米粉体为吸附剂,研究了HAp纳米粉体对水溶液中酚类物质的吸附分离性能。探讨了吸附时间、pH值、苯酚初始浓度、吸附剂浓度、吸附温度和吸附剂煅烧温度对苯酚吸附效果的影响规律;研究了取代基对吸附效果的影响规律,以及吸附动力学、吸附等温线方程和吸附热力学。研究结果表明HAp材料可以较好地吸附去除溶液中的酚类化合物,有望作为一种新型的、生物相容性和环境友好的酚类污染物吸附分离试剂,具有良好的应用前景。
以上研究结果显示,采用纳米粉体可以制备得到力学性能良好的磷酸钙、硅酸钙及其复合生物陶瓷材料;通过改变磷酸钙和硅酸钙的复合比例,可以对磷酸钙/硅酸钙纳米复合陶瓷材料的力学性能、生物活性和降解性进行调节;多孔硅酸钙生物陶瓷材料具有良好的力学性能、生物相容性、生物活性、体内降解性和骨修复性能,有望用于硬组织修复和骨组织工程用支架领域;纳米HAp粉体对酚类物质具有良好的吸附分离性能,有望作为一种新型的、生物相容性和环境友好的酚类污染物吸附分离试剂,并具有良好的应用前景。
In this study,theβ-tricalcium phosphate(β-Ca_3(PO_4)_2,β-TCP)nanopowders, hydroxyapatite(Ca_(10)(PO_4)_6(OH)_2,HAp)nanopowders,tobermorite (Ca_5Si_6O_(16)(OH)_2·4H_2O)nanowires,xonotlite(Ca_6Si_6O_(17)(OH)_2)nanowires,calcium silicate(CaSiO_3,CS)ultrafine powders and nanowires,β-TCP/CS and HAp/CS composite nanopowders were prepared.The bioactivity and degradability of tobermorite nanowires in vitro were investigated.The sintering ability of the apatite nanopowders and calcium silicate nanopowders,and the properties of the sintered matrixes were performed.Theβ-TCP/CS and HAp/CS composite nanoceramics were developed,and the mechanical properties,bioactivity(bone-like apatite-formation ability in vitro)and in vitro dissolution behavior of the fabricated samples with different composite ratios were examined.The macroporousβ-TCP and CS ceramic scaffolds with high mechanical strength and the novel porous samples similar to the natural bone structures were explored,and the biocompatibility,bioactivity, degradability and in vivo bone-regenerative capacity of the scaffolds were investigated.Furthermore,the adsorption of phenolic pollutants on HAp nanopowders was studied.The obtained results are described as followings:
1.(1)The HAp nanopowders with different morphologies,crystallinity,particle size and specific surface area could be obtained using chemical precipitation method, hydrothermal microemulison method,ultrasonic chemical method or homogeneous-precipitation method.(2)Theβ-TCP nanopowders with 80～100nm could be obtained in large-scale by chemical precipitation method.(3)The monodispersed tobermorite nanowires with diameter of 30～50nm and up to tens of micrometers in length were prepared via hydrothermal microemulsion method.(4) The monodispersed xonotlite nanowires with diameter of 10～30nm and up to tens of micrometers in length were prepared via a simple hydrothermal method.After calcining at 800℃for 2h,xonotlite nanowires completely transformed intoβ-wollastonite nanowires and the wire-like structure and sizes were also preserved.(5) Theβ-TCP/CS and HAp/CS composite nanopowders with different composite ratios and well dispersions were synthesized by two-step chemical precipitation method. The particle sizes ofβ-TCP/CS and HAp/CS composite nanopowders were 20～80nm and 10～30nm,respectively.
2.In vitro bioactivity of the tobermorite nanofibers was evaluated by examing the bone-like HAp forming ability on the surface after soaking in simulated body fluid (SBF)for various periods.After soaking in SBF for 3d,the nanofibers were completely covered by bonelike hydroxycarbonate apatite(HCA)layers,and the nanofibers after soaking still kept stability in fibrous morphology.The dissolution of the nanofibers reached about 24.5%after soaking in SBF for 14d.The results suggested that the tobermorite nanofibers exhibited certain desirable characteristics including bioactivity,degradability and stability in morphology,and a potential candidate as reinforcement materials to develop novel bioactive and degradable composites for biomedical applications.On the other hand,the tobermorite nanofibers might be used as the alkaline biodegradability materials to fabricate the composite biomaterials,which might not only contribute to the improved bioactivity of those acid biodegradability polymer materials,but also be able to neutralize the acidic degradation products of the polymers.
3.Using the nanopowders as raw materials,the apatite and calcium silicate bioceramics were fabricated by sintering green compacts at atmosphere after cold isostatic pressure respectively.The results showed that the nanopowders possessed excellent sintering ability,and the ceramic samples with ultrafine crystal size and high densities could be obtained.Therefore,the apatite and calcium silicate bioceramics with well mechanical strength could be fabricated using nano-sized powders.(1)β-TCP bioceramics with high mechanical strength of 200MPa were fabricated using the nano-size powders,which were more than two times higher as compared to those of samples fabricated from micro-size powders.(2)The transparentβ-TCP bioceramics were fabricated using nano-size powders and(Spark Plasma Sintering, SPS).The transparent bodies had an average grain size of 250nm.The transparency of the samples with 1.0mm thickness reached about 52%.The MTT method showed that the proliferation of bone mesenchymal stem cells on transparentβ-TCP bioceramics was much better than that on the polystyrene cell culture cluster,suggesting that the transparentβ-TCP may be used as cell carrier materials and window materials for biomedical applications.(3)The dense HAp nanoceramics with an average grain size of 193nm were obtained through two-step sintering method.The fracture toughness reached 1.18MPa·m~(1/2),which was about 60%higher than that of the samples with an average grain size of 765nm and fabricated by normal sintering method.(4)The bending strength of the CaSiO_3 bioceramics sintered from nanowires reached about 146MPa,which was similar to the upper value of the human cortical bones and was 53%higher than that of the samples sintered from superfine powders.The elastic modul of the fabricated CaSiO_3 bioceramics was similar to the human cortical bone. The study showed that the CaSiO_3 bioceramics with well mechanical strength could be fabricated using nanowires as raw materials.(5)The CaSiO_3 bioceramics possessed excellent bioactivity,degradability and cell compatibility.After soaking in SBF for 1d,the samples were completely covered by bonelike HAp layers.The dissolution ratio of the ceramics reached about 27.85%after soaking in Tris-HCl buffer solution for 28d,which was much higher than that ofβ-TCP bioceramics.The adhesion and proliferation of bone marrow mesenchymal stem cells on the CaSiO_3 ceramics was examined and the results showed that the ceramics supported cell adhesion and proliferation,which indicated good biocompatibility.Our results suggested that CaSiO_3 ceramics might be a potential bioactive and degradable material as bone implant.
4.Using the nano-composite powders as raw materials,theβ-TCP/CS composite nanoceramics have been fabricated by sintering green compacts at atmosphere after cold isostatic pressure.The mechanical strength,bioactivity and degradability of the composite ceramics could be regulated by the composite ratios.The bending strength of the samples withβ-TCP component higher than 50wt.%was similar to the bending strength of human cortical bone.The mechanical strength increased with the increase of theβ-TCP component amount.The composite ceramics showed excellent bioactivity when the CS component ratio was higher than 30wt.%.After soaking in SBF for 1d,the samples were completely covered by bonelike HAp layers.The bioactivity and degradability increased with the increase of the CS component amount.
5.Using the nano-composite powders as raw materials,the HAp/CS composite nanoceramics have been fabricated by sintering green compacts at atmosphere after cold isostatic pressure.The mechanical strength,bioactivity and degradability of the composite ceramics could be regulated by the composite ratios.The bending strength of the samples was in the range of 98.06 and 221.30MPa,and the elastic modul of the fabricated nanocomposite bioceramics was similar to the human cortical bone.The bending strength of the samples with CS component over 50wt.%was higher than the bending strength of human cortical bone.The mechanical strength,bioactivity and degradability increased with the increase of the CS component amount.
6.The macroporousβ-TCP and CS scaffolds were successfully fabricated by porogen burning-out method,casting method and polymer sponge method.The results showed that the scaffolds with well mechanical strength could be obtained by the porogen burning-out method and the casting method.And the structure of the scaffolds fabricated by the polymer sponge method was open and interconnected pores,which showed that the structure of the scaffolds was similar to that of natural cancellous bones.Furthermore,theβ-TCP scaffolds with high mechanical strength could be fabricated from the nano-size powders.After soaking in SBF for 1d,the CS scaffolds were completely covered by HCA layers.The degradability of the CS samples with porosity of 63.1%reached 7.14%after soaking in SBF for 7d.The results suggested excellent in vitro bioactivity and degradability of the macroporous CS scaffolds.Therefore,the CS scaffolds may be potential candidates as bioactive and degradable scaffolds for hard tissue repair and bone tissue engineering applications.
7.Theβ-TCP and CS scaffolds were implanted in rabbit subcutaneous sites and the rabbit calvarial defect sites,respectively to investigate the biological characteristics,in vivo bone-regenerative capacity and resorption of the materials. Compared withβ-TCP,the results showed that the CS scaffolds possessed superiority in vascularization,ingrowth of new tissue,degradation and bone-regenerative ability in early stage.The TRAP-positive multinucleated cells were observed on the surface ofβ-CS,suggested a cell-mediated process involved in the degradation ofβ-CS in vivo.Histological observation demonstrated that newly formed bone tissue grew into the porousβ-CS,and a bone-like HAp layer was identified between the bone tissue and CS materials.The studies showed that the CS scaffolds could stimulate bone regeneration and may be used as bioactive and biodegradable materials for hard tissue repair and bone tissue engineering applications.
8.The HAp nanopowders were used as the adsorbent,and the potential of HAp nanopowders for phenolic pollutant adsorption from aqueous solution was studied. The effect of contact time,initial phenol concentration,pH,adsorbent dosage, solution temperature and adsorbent calcining temperature on the phenol adsorption, and the adsorption kinetic,equilibrium and thermodynamic parameters of phenolic pollutants were investigated.The results showed that the HAp nanopowders possessed good adsorption ability to phenolic pollutants.The results suggested that the HAp nanopowders might be a new potential,biocompatible and good adsorbent for the removal of phenol pollutants from aqueous solutions.
In conclusion,the apatite,calcium silicate and their composite bioceramics could be fabricated using the nano-size powders as the raw materials.The mechanical strength,bioactivity and degradability of theβ-TCP/CS and HAp/CS composite nanoceramics could be regulated by the composite ratios.The CS scaffolds possessed excellent biocompatibility,bioactivity,biodegradability and bone-regenerative ability, and may be used as bioactive and biodegradable materials for hard tissue repair and bone tissue engineering applications.The HAp nanopowders possessed good adsorption ability to phenolic pollutants,and may be a new potential,biocompatible and good adsorbent for the removal of phenol pollutants from aqueous solutions.
1、(1)应用化学沉淀法、水热微乳液法、超声化学法和水热均相沉淀法,并通过控制工艺条件可以制备得到不同形貌、结晶度、颗粒尺寸和比表面积的HAp纳米粉体;(2)采用化学沉淀法可以规模化制备得到颗粒尺寸约80～100nm的β-TCP纳米粉体;(3)采用水热微乳液法制备得到分散性良好的、颗粒细小且晶粒尺寸分布窄的Tobermorite纳米线,纳米线的直径约30～50nm,长度最高达10多微米;(4)采用简单的水热处理法制备了分散性良好的Xonotlite纳米线,粉体直径约10～30nm、长度可以达10多微米,Xonotlite纳米线于800℃煅烧2h获得CS纳米线,粉体的形貌和尺寸基本保持不变;(5)采用两步化学沉淀法制备得到复合比例可控的、分散性良好的β-TCP/CS和HAp/CS纳米复合粉体,粉体颗粒尺寸分别为20～80nm和10～30nm。
2、研究了Tobermorite纳米线的体外生物活性和降解性。研究表明Tobermorite纳米线在模拟体液(Simulated body fluid,SBF)中具有良好的生物活性(诱导沉积类骨HAp的能力)和降解性。在SBF中浸泡3d,表面即完全被类骨HAp覆盖;14d的降解率达24.5wt.%。Tobermorite纳米线降解后溶液介质的pH明显升高,该性能使其可被应用于中和聚酯类生物高分子的酸性降解产物,以避免这类传统高分子材料因降解产生的酸性产物而引发的无菌性炎症反应。研究结果显示Tobermorite纳米线有望作为良好的可降解生物活性增强体应用于制备生物活性复合材料。
3、以纳米粉体为原料,采用干压、冷等静压成型技术,通过控制烧结工艺制备了磷酸钙和硅酸钙生物陶瓷材料。研究表明纳米粉体具有良好的烧结活性,并可以制备得到晶粒细小的、高致密度的烧结体,从而获得力学性能良好的磷酸钙和硅酸钙生物陶瓷材料:(1)采用常规无压烧结工艺制备了高强度的β-TCP生物陶瓷,其抗弯强度高达200MPa,是微米粉体烧结体的2倍,且明显高于文献报道的结果。(2)采用放电等离子体烧结工艺(Spark PlasmaSintering,SPS)制备得到透明β-TCP生物陶瓷,平均晶粒尺寸约250 nm,具有良好的透光性能、最大透光率约52%(1mm厚)。细胞相容性研究结果表明,透明β-TCP生物陶瓷对骨髓间质干细胞的增殖作用明显高于常规的通用聚乙烯培养板,可望作为新型的细胞培养载体材料和医学窗口材料。(3)常压下,采用简单的两步烧结工艺(Two-step Sintering Method,TSM)制备得到平均晶粒尺寸为193nm的致密HAp纳米生物陶瓷材料,其晶粒尺寸明显低于传统的无压烧结工艺(高达765nm),TSM制备得到的HAp纳米生物陶瓷材料的韧性达1.18MPa·m~(1/2),较无压烧结工艺提高了约60%。(4)采用CS纳米线于1100℃无压烧结3h可以获得抗弯强度约146MPa、与人体皮质骨强度的上限值相当,其强度较CS超细粉体烧结体提高了约53%,而弹性模量也与人体致密骨相当。研究结果表明采用纳米线有望获得力学强度较好的CS生物陶瓷材料。(5)CS生物陶瓷具有良好的生物活性、降解性和细胞相容性,在SBF中浸泡1d后即可在表面沉积一层类骨HAp层,表明材料具有良好的生物活性,在Tris-HCl缓冲液浸泡28d的降解率达27.85%、远高于β-TCP的降解率(仅2.51%),骨髓间质干细胞的贴壁和增殖实验表明CS陶瓷具有良好的生物相容性。研究结果表明CS生物陶瓷材料有望作为新型的可降解生物活性骨修复材料。
4、以纳米复合粉体为原料,采用干压、冷等静压成型技术,并采用无压烧结工艺制备了β-TCP/CS纳米复合生物陶瓷材料。研究表明复合生物陶瓷的力学性能、生物活性和降解性可以通过复合比例加以有效调控。当β-TCP的复合比例高于50wt.%时,即可制备得到力学强度与人体皮质骨相当的复合生物陶瓷材料,且强度随β-TCP复合比例的提高明显升高;而当CS的复合比例超过30wt.%时,材料即显示优越的生物活性,在SBF中浸泡1d即完全被类骨HAp层覆盖,且复合陶瓷的生物活性和降解性随CS组分的含量增加而提高。
5、以纳米复合粉体为原料,采用干压、冷等静压成型技术,并采用无压烧结工艺制备了CS/HAp纳米复合生物陶瓷材料。研究表明复合生物陶瓷的力学性能、生物活性和降解性可以通过复合比例加以有效调控。通过调节复合比例,CS/HAp复合陶瓷的抗弯强度可以控制在98.06～221.30MPa,当CS复合比例高于50wt.%时,材料的强度显著高于人体皮质骨,而弹性模量与人体致密骨相当。复合陶瓷的生物活性和降解性随CS组分含量的提高而增强。
6、采用添加造孔剂法、注浆成型工艺和泡沫浸渍工艺制备了多孔β-TCP和CS生物陶瓷支架材料。实验表明采用添加造孔剂法和注浆成型工艺制备得到的材料力学强度较好,采用注浆成型工艺和泡沫浸渍工艺可以获得孔连通性良好的多孔陶瓷支架材料,而采用泡沫浸渍工艺还可以获得与天然松质骨结构相类似的多孔陶瓷支架材料。同时,采用纳米粉体可以制备得到力学强度良好的β-TCP多孔陶瓷支架材料。SBF浸泡实验表明,CS支架在SBF中浸泡1d表面就全部被类骨HAp层覆盖住,同时支架材料具有良好的降解性,气孔率为63.1%的支架材料7d的降解率达7.14%。研究结果表明多孔CS生物陶瓷支架材料有望作为新型的可降解生物活性骨修复材料和骨组织工程支架材料。
7、研究了多孔β-CS和CS生物陶瓷支架材料的非骨性环境下的生物学行为、以及兔子颅骨的缺损修复性能。研究表明,多孔CS生物陶瓷在早期血管化、新生组织长入、材料降解性和骨修复能力等方面均较传统的β-TCP生物陶瓷具有明显优势。动物植入实验还表明细胞调节作用参与了CS材料的体内降解过程;SEM和EDS分析结果表明新生骨生成于CS材料诱导沉积的类骨HAp层表面,而不是直接作用于CS材料表面,表明生成的类骨HAp层对新骨的生成、以及材料同骨组织的键合作用起关键作用。动物植入试验研究结果表明,多孔CS陶瓷材料有望作为可降解生物活性材料应用于硬组织修复和骨组织工程材料领域。
8、以HAp纳米粉体为吸附剂,研究了HAp纳米粉体对水溶液中酚类物质的吸附分离性能。探讨了吸附时间、pH值、苯酚初始浓度、吸附剂浓度、吸附温度和吸附剂煅烧温度对苯酚吸附效果的影响规律;研究了取代基对吸附效果的影响规律,以及吸附动力学、吸附等温线方程和吸附热力学。研究结果表明HAp材料可以较好地吸附去除溶液中的酚类化合物,有望作为一种新型的、生物相容性和环境友好的酚类污染物吸附分离试剂,具有良好的应用前景。
以上研究结果显示,采用纳米粉体可以制备得到力学性能良好的磷酸钙、硅酸钙及其复合生物陶瓷材料;通过改变磷酸钙和硅酸钙的复合比例,可以对磷酸钙/硅酸钙纳米复合陶瓷材料的力学性能、生物活性和降解性进行调节;多孔硅酸钙生物陶瓷材料具有良好的力学性能、生物相容性、生物活性、体内降解性和骨修复性能,有望用于硬组织修复和骨组织工程用支架领域;纳米HAp粉体对酚类物质具有良好的吸附分离性能,有望作为一种新型的、生物相容性和环境友好的酚类污染物吸附分离试剂,并具有良好的应用前景。
In this study,theβ-tricalcium phosphate(β-Ca_3(PO_4)_2,β-TCP)nanopowders, hydroxyapatite(Ca_(10)(PO_4)_6(OH)_2,HAp)nanopowders,tobermorite (Ca_5Si_6O_(16)(OH)_2·4H_2O)nanowires,xonotlite(Ca_6Si_6O_(17)(OH)_2)nanowires,calcium silicate(CaSiO_3,CS)ultrafine powders and nanowires,β-TCP/CS and HAp/CS composite nanopowders were prepared.The bioactivity and degradability of tobermorite nanowires in vitro were investigated.The sintering ability of the apatite nanopowders and calcium silicate nanopowders,and the properties of the sintered matrixes were performed.Theβ-TCP/CS and HAp/CS composite nanoceramics were developed,and the mechanical properties,bioactivity(bone-like apatite-formation ability in vitro)and in vitro dissolution behavior of the fabricated samples with different composite ratios were examined.The macroporousβ-TCP and CS ceramic scaffolds with high mechanical strength and the novel porous samples similar to the natural bone structures were explored,and the biocompatibility,bioactivity, degradability and in vivo bone-regenerative capacity of the scaffolds were investigated.Furthermore,the adsorption of phenolic pollutants on HAp nanopowders was studied.The obtained results are described as followings:
1.(1)The HAp nanopowders with different morphologies,crystallinity,particle size and specific surface area could be obtained using chemical precipitation method, hydrothermal microemulison method,ultrasonic chemical method or homogeneous-precipitation method.(2)Theβ-TCP nanopowders with 80～100nm could be obtained in large-scale by chemical precipitation method.(3)The monodispersed tobermorite nanowires with diameter of 30～50nm and up to tens of micrometers in length were prepared via hydrothermal microemulsion method.(4) The monodispersed xonotlite nanowires with diameter of 10～30nm and up to tens of micrometers in length were prepared via a simple hydrothermal method.After calcining at 800℃for 2h,xonotlite nanowires completely transformed intoβ-wollastonite nanowires and the wire-like structure and sizes were also preserved.(5) Theβ-TCP/CS and HAp/CS composite nanopowders with different composite ratios and well dispersions were synthesized by two-step chemical precipitation method. The particle sizes ofβ-TCP/CS and HAp/CS composite nanopowders were 20～80nm and 10～30nm,respectively.
2.In vitro bioactivity of the tobermorite nanofibers was evaluated by examing the bone-like HAp forming ability on the surface after soaking in simulated body fluid (SBF)for various periods.After soaking in SBF for 3d,the nanofibers were completely covered by bonelike hydroxycarbonate apatite(HCA)layers,and the nanofibers after soaking still kept stability in fibrous morphology.The dissolution of the nanofibers reached about 24.5%after soaking in SBF for 14d.The results suggested that the tobermorite nanofibers exhibited certain desirable characteristics including bioactivity,degradability and stability in morphology,and a potential candidate as reinforcement materials to develop novel bioactive and degradable composites for biomedical applications.On the other hand,the tobermorite nanofibers might be used as the alkaline biodegradability materials to fabricate the composite biomaterials,which might not only contribute to the improved bioactivity of those acid biodegradability polymer materials,but also be able to neutralize the acidic degradation products of the polymers.
3.Using the nanopowders as raw materials,the apatite and calcium silicate bioceramics were fabricated by sintering green compacts at atmosphere after cold isostatic pressure respectively.The results showed that the nanopowders possessed excellent sintering ability,and the ceramic samples with ultrafine crystal size and high densities could be obtained.Therefore,the apatite and calcium silicate bioceramics with well mechanical strength could be fabricated using nano-sized powders.(1)β-TCP bioceramics with high mechanical strength of 200MPa were fabricated using the nano-size powders,which were more than two times higher as compared to those of samples fabricated from micro-size powders.(2)The transparentβ-TCP bioceramics were fabricated using nano-size powders and(Spark Plasma Sintering, SPS).The transparent bodies had an average grain size of 250nm.The transparency of the samples with 1.0mm thickness reached about 52%.The MTT method showed that the proliferation of bone mesenchymal stem cells on transparentβ-TCP bioceramics was much better than that on the polystyrene cell culture cluster,suggesting that the transparentβ-TCP may be used as cell carrier materials and window materials for biomedical applications.(3)The dense HAp nanoceramics with an average grain size of 193nm were obtained through two-step sintering method.The fracture toughness reached 1.18MPa·m~(1/2),which was about 60%higher than that of the samples with an average grain size of 765nm and fabricated by normal sintering method.(4)The bending strength of the CaSiO_3 bioceramics sintered from nanowires reached about 146MPa,which was similar to the upper value of the human cortical bones and was 53%higher than that of the samples sintered from superfine powders.The elastic modul of the fabricated CaSiO_3 bioceramics was similar to the human cortical bone. The study showed that the CaSiO_3 bioceramics with well mechanical strength could be fabricated using nanowires as raw materials.(5)The CaSiO_3 bioceramics possessed excellent bioactivity,degradability and cell compatibility.After soaking in SBF for 1d,the samples were completely covered by bonelike HAp layers.The dissolution ratio of the ceramics reached about 27.85%after soaking in Tris-HCl buffer solution for 28d,which was much higher than that ofβ-TCP bioceramics.The adhesion and proliferation of bone marrow mesenchymal stem cells on the CaSiO_3 ceramics was examined and the results showed that the ceramics supported cell adhesion and proliferation,which indicated good biocompatibility.Our results suggested that CaSiO_3 ceramics might be a potential bioactive and degradable material as bone implant.
4.Using the nano-composite powders as raw materials,theβ-TCP/CS composite nanoceramics have been fabricated by sintering green compacts at atmosphere after cold isostatic pressure.The mechanical strength,bioactivity and degradability of the composite ceramics could be regulated by the composite ratios.The bending strength of the samples withβ-TCP component higher than 50wt.%was similar to the bending strength of human cortical bone.The mechanical strength increased with the increase of theβ-TCP component amount.The composite ceramics showed excellent bioactivity when the CS component ratio was higher than 30wt.%.After soaking in SBF for 1d,the samples were completely covered by bonelike HAp layers.The bioactivity and degradability increased with the increase of the CS component amount.
5.Using the nano-composite powders as raw materials,the HAp/CS composite nanoceramics have been fabricated by sintering green compacts at atmosphere after cold isostatic pressure.The mechanical strength,bioactivity and degradability of the composite ceramics could be regulated by the composite ratios.The bending strength of the samples was in the range of 98.06 and 221.30MPa,and the elastic modul of the fabricated nanocomposite bioceramics was similar to the human cortical bone.The bending strength of the samples with CS component over 50wt.%was higher than the bending strength of human cortical bone.The mechanical strength,bioactivity and degradability increased with the increase of the CS component amount.
6.The macroporousβ-TCP and CS scaffolds were successfully fabricated by porogen burning-out method,casting method and polymer sponge method.The results showed that the scaffolds with well mechanical strength could be obtained by the porogen burning-out method and the casting method.And the structure of the scaffolds fabricated by the polymer sponge method was open and interconnected pores,which showed that the structure of the scaffolds was similar to that of natural cancellous bones.Furthermore,theβ-TCP scaffolds with high mechanical strength could be fabricated from the nano-size powders.After soaking in SBF for 1d,the CS scaffolds were completely covered by HCA layers.The degradability of the CS samples with porosity of 63.1%reached 7.14%after soaking in SBF for 7d.The results suggested excellent in vitro bioactivity and degradability of the macroporous CS scaffolds.Therefore,the CS scaffolds may be potential candidates as bioactive and degradable scaffolds for hard tissue repair and bone tissue engineering applications.
7.Theβ-TCP and CS scaffolds were implanted in rabbit subcutaneous sites and the rabbit calvarial defect sites,respectively to investigate the biological characteristics,in vivo bone-regenerative capacity and resorption of the materials. Compared withβ-TCP,the results showed that the CS scaffolds possessed superiority in vascularization,ingrowth of new tissue,degradation and bone-regenerative ability in early stage.The TRAP-positive multinucleated cells were observed on the surface ofβ-CS,suggested a cell-mediated process involved in the degradation ofβ-CS in vivo.Histological observation demonstrated that newly formed bone tissue grew into the porousβ-CS,and a bone-like HAp layer was identified between the bone tissue and CS materials.The studies showed that the CS scaffolds could stimulate bone regeneration and may be used as bioactive and biodegradable materials for hard tissue repair and bone tissue engineering applications.
8.The HAp nanopowders were used as the adsorbent,and the potential of HAp nanopowders for phenolic pollutant adsorption from aqueous solution was studied. The effect of contact time,initial phenol concentration,pH,adsorbent dosage, solution temperature and adsorbent calcining temperature on the phenol adsorption, and the adsorption kinetic,equilibrium and thermodynamic parameters of phenolic pollutants were investigated.The results showed that the HAp nanopowders possessed good adsorption ability to phenolic pollutants.The results suggested that the HAp nanopowders might be a new potential,biocompatible and good adsorbent for the removal of phenol pollutants from aqueous solutions.
In conclusion,the apatite,calcium silicate and their composite bioceramics could be fabricated using the nano-size powders as the raw materials.The mechanical strength,bioactivity and degradability of theβ-TCP/CS and HAp/CS composite nanoceramics could be regulated by the composite ratios.The CS scaffolds possessed excellent biocompatibility,bioactivity,biodegradability and bone-regenerative ability, and may be used as bioactive and biodegradable materials for hard tissue repair and bone tissue engineering applications.The HAp nanopowders possessed good adsorption ability to phenolic pollutants,and may be a new potential,biocompatible and good adsorbent for the removal of phenol pollutants from aqueous solutions.
引文
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