本文選題：納米羥基磷灰石 + 聚己內(nèi)酯��； 參考：《安徽大學》2012年碩士論文

【摘要】：生物支架材料一直都是組織工程領域研究的主要內(nèi)容之一。幾乎所有的具有可生物降解性,無論天然大分子和合成高分子生物材料均可用于不同組織工程支架研究。近年來,發(fā)展了如熱致相分離法、致孔劑法、靜電紡絲法等十余種組織工程的制備技術(shù)。其中,靜電紡絲法由于能夠直接制備連續(xù)的聚合物納米纖維,因此有其獨特的優(yōu)勢。電紡制備的納米纖維支架結(jié)構(gòu)類似于細胞間質(zhì),有利于細胞的粘附增殖。目前,電紡纖維支架材料已經(jīng)廣泛應用于各種組織工程的研究,尤其是骨組織工程方面。 本文采用水熱合成法,成功制備了尺寸為20-30nm×50-70nm的棒狀nHA,并利用nHA活性粉體引發(fā)ε-CL單體聚合,成功合成了nHA含量不同的nHA-PCL復合材料。取nHA含量為5%的nHA-PCL-3作為樣品,對nHA-PCL復合材料的電紡條件進行調(diào)試和選擇。對于電紡溶劑的選擇,主要研究了DCM和DMF體積比分別為1：1和2：1、DCM與甲酸體積比為1：1和2：1的四種混合溶劑。SEM結(jié)果顯示：DCM和DMF的2種比例的混合溶劑電紡后得到的膜纖維交聯(lián)嚴重、纖維無法獨立呈現(xiàn)；而DCM和甲酸的混合溶劑電紡所得膜纖維的形貌好許多,尤其當體積比為2：1時的混合溶劑,膜纖維的粗細較均勻、纖維可以獨立呈現(xiàn)；因而最終選擇DCM和甲酸體積比為2：1的混合溶劑作為nHA-PCL復合材料的電紡溶劑。另外,在其他條件一致、單一因素改變的情況下,還對材料的不同的電紡濃度、電紡電壓和接收距離進行實驗。通過SEM圖片看出,nHA-PCL復合材料的電紡濃度應控制在20%左右,適宜的電紡電壓和接收距離分別為15kV和15cm。 在選擇合適的電紡條件后,成功制備出不同nHA含量的nHA-PCL的復合電紡膜,并對nHA-PCL復合電紡膜的結(jié)構(gòu)和性能進行分析。SEM結(jié)果顯示,電紡膜的纖維的直徑隨著nHA含量提高而降低；其中nHA含量為1%、3%和5%的復合電紡膜的纖維形貌較好,但含量為7%的nHA-PCL-4復合電紡膜,由于nHA顆粒的團聚,纖維粗細不均勻、連續(xù)性差、膜表面粗糙。從FT-IR和DSC的結(jié)果得到,電紡后的nHA-PCL復合材料較電紡前結(jié)品度有明顯的提高,說明了nHA-PCL復合材料在強電力的拉伸作用下,分子鏈會沿著被拉伸方向取向,使得復合材料可以在纖維固化之前得到較充分的結(jié)品。此外,由于各nHA-PCL復合電紡膜的結(jié)品度的不同,表現(xiàn)在材料的力學性能也有所差異,其中當nHA含量為5%時的nHA-PCL-3復合電紡膜的力學性能最好,其拉伸強度和斷裂伸長率分別為29.2±1.1MPa和55.6士1.5%。為研究nHA-PCL復合電紡膜的骨誘導性,將復合電紡膜放于1.5倍的SBF中浸泡,當浸泡7天后,各個電紡膜的纖維表面均有不同程度的沉積物形成； 其中FT-IR結(jié)果顯示,該沉積物主要成分為磷灰石,且隨著nHA含量的提高,nHA-PCL電紡膜的磷灰石沉積量有所增加；另外,礦化后的復合電紡膜還表現(xiàn)在接觸角比較礦化前有大幅度降低,說明礦化后的nHA-PCL電紡膜的親水性良好。 為了比較純PCL和不同復合方式得到的nHA與PCL復合電紡材料的性能,對購買的純PCL、物理共混nHA/PCL和化學接枝nHA-PCL的3種電紡膜進行研究。FT-IR、 DSC、SEM等的測試均表明了,含量均為5%的nHA在nHA-PCL中較nHA/PCL分散好,因此nHA在前者中異相成核點的作用較強,表現(xiàn)在前者的PCL結(jié)晶性能不僅高于后者,且還高于純的PCL電紡膜；此外,nHA-PCL復合電紡膜的熱穩(wěn)定性及力學性能也明顯高于另外兩者。在1.5倍SBF仿生礦化實驗結(jié)果顯示,相同時間內(nèi)nHA-PCL電紡膜纖維表面磷灰石的生成量明顯高于nHA/PCL共混物電紡膜和純PCL電紡膜,顯示出良好的生物成骨性能。
[Abstract]:Biological scaffolds have been one of the main contents of the research in the field of tissue engineering. Almost all of them have biodegradability, both natural macromolecules and synthetic polymer biomaterials can be used in the study of different tissue engineering scaffolds. In recent years, more than ten kinds of tissues such as thermal phase separation, pore forming agent, electrospinning and so on have been developed. The electrostatic spinning method has its unique advantages because it can directly prepare the continuous polymer nanofibers. The structure of the nanofiber scaffold prepared by electrospinning is similar to the cell interstitium and is beneficial to the cell adhesion and proliferation. Especially in bone tissue engineering.
In this paper, a rod like nHA with a size of 20-30nm x 50-70nm was successfully prepared by hydrothermal synthesis. The nHA-PCL composite with different nHA content was successfully synthesized by using nHA active powder to induce the monomer -CL monomer polymerization. A nHA-PCL-3 of nHA content of 5% was taken as a sample, and the electrospun conditions of the nHA-PCL composite were tested and selected. The choice of DCM and DMF volume ratio of 1:1 and 2:1, DCM and formic acid volume ratio of 1:1 and 2:1 four kinds of mixed solvent.SEM results show that the 2 proportion of DCM and DMF mixed solvent electrospun is serious, fiber can not be independently presented; DCM and formic acid mixed solvent electrospun membrane fiber The morphology of the dimension is much better, especially when the volume ratio is 2:1, the thickness of the membrane fiber is more uniform and the fiber can be presented independently. Thus, the mixed solvent of DCM and the volume ratio of formic acid to 2:1 is selected as the electrospun solvent of the nHA-PCL composite. Different electrospun concentration, electrospun voltage and receiving distance are tested. Through SEM images, it is found that the electrospun concentration of nHA-PCL composites should be controlled at about 20%, and the suitable electrospun voltage and receiving distance are 15kV and 15cm., respectively.
After selecting suitable electrospinning conditions, the composite electrospun membranes with different nHA content of nHA-PCL were successfully prepared and the structure and properties of nHA-PCL composite electrospun membranes were analyzed..SEM results showed that the diameter of the fibers of the electrospun membranes decreased with the increase of nHA content, and the fiber morphology of the composite electrospun membranes with nHA content of 1%, 3% and 5% was better, but the morphology of the fiber was better. The nHA-PCL-4 composite electrospun membrane with a content of 7%, because of the agglomeration of nHA particles, the roughness of the fiber is not uniform, the continuity is poor, the surface of the membrane is rough. From the results of FT-IR and DSC, the nHA-PCL composite material after electrospun is obviously improved compared with the electrospinning. It shows that the molecular chain will be dragged along the tensile force of the strong electric power. In addition, the mechanical properties of the nHA-PCL composite electrospun membranes are different. In addition, the mechanical properties of the nHA-PCL-3 composite electrospun membranes with nHA content of 5% are the best, and the tensile strength and elongation at break are the best. The rate of 29.2 + 1.1MPa and 55.6 St 1.5%. was the bone inducibility of the nHA-PCL composite electrospun membrane. The composite electrospun membranes were soaked in 1.5 times of SBF, and the surface of the fibers of the electrospun membranes were formed in different degrees of sediment when they were soaked.
FT-IR results show that the main component of the deposit is apatite, and the amount of apatite in the nHA-PCL electrospun membrane increases with the increase of the content of nHA. In addition, the composite electrospun membrane after mineralization is also greatly reduced before the contact angle is mineralized, indicating that the hydrophilic property of the nHA-PCL electrospun membrane after mineralization is good.
In order to compare the properties of nHA and PCL composite electrospun materials obtained by pure PCL and different composite methods, 3 kinds of electrospun membranes purchased pure PCL, physical blending nHA/PCL and chemical grafting nHA-PCL were studied.FT-IR, DSC, SEM and other tests showed that nHA in the nHA-PCL 5% was better than nHA/PCL dispersed in nHA-PCL. The effect of the point is stronger than that of the former, which is not only higher than the latter, but also higher than the pure PCL electrospun membrane. In addition, the thermal stability and mechanical properties of the nHA-PCL composite electrospun membrane are obviously higher than that of the other two. The results of the 1.5 times SBF biomimetic mineralization experiment show that the formation of apatite on the surface of nHA-PCL electrospun fiber surface within the same time is at the same time. It is obviously higher than that of nHA/PCL blend electrospinning film and pure PCL electrospinning film, showing good biological osteogenic property.
【學位授予單位】：安徽大學
【學位級別】：碩士
【學位授予年份】：2012
【分類號】：R318.08

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