3D打印Ti-6Al-4V理化性能及生物相容性研究

发布时间：2018-06-24 16:34

本文选题：选区激光熔化(SLM) + 电子束选区熔化(EBM)　；参考：《中国人民解放军医学院》2016年博士论文

【摘要】：[目的]检测、比较应用电子束选区熔化(EBM)及激光选区熔化(SLM)工艺制作的Ti-6A1-4V试件的理化性能和生物相容性,为3D打印钛合金的临床应用提供理论依据[方法]理化性能：应用电子束选区熔化(EBM)和激光选区熔化(SLM)工艺制备Ti-6A1-4V合金试件,以锻造试件作为对照。(1)通过光学显微镜、扫描电镜、透射电镜、EBSD的方法观察显微组织；(2)通过XRD、EDS、XPS和GB/T4698系列方法对其进行成分分析；(3)运用接触角实验方法检测EBM和SLM试件亲水性；(4)应用维氏硬度方法检测三种试件的维氏硬度。(5)应用粗糙度仪检测EBM和SLM试件表面粗糙度;(6)应用电化学实验、浸泡实验、细胞培养液离子析出实验方法检测其耐腐蚀性。生物相容性：体外研究为EBM、SLM及锻造三者比较。体内研究为EBM与正常组织比较。(1)应用扫描电镜及细胞计数的方法观察,不同时间点骨髓基质干细胞(BMSC)在不同工艺制备的试件上粘附、增殖情况。(2)应用透射电镜的方法观察粘附在不同工艺试件上的BMSC及进行皮下植入手术52周后的比格犬肝、肾组织超微结构是否有损伤。(3)应用组织学染色及大体观察方法观察Ti-6A1-4V试件周围组织有无异常。(4)应用单细胞电泳实验(彗星实验)检测进行皮下植入手术52周后的比格犬肝、肾组织DNA是否有损伤。[结果]理化性能：显微组织观察结果表明：三种试件的显微结构均不同。锻造试件为网篮组织,EBM与SLM均为马氏体组织,大部分SLM的晶粒较EBM细小。在SLM试件中发现很多短小的位错及孪晶。在EBM试件中发现有金属间化合物析出。从表面粗糙度结果可知：EBM和SLM表面粗糙度均有利于细胞的粘附。接触角实验结果表明：EBM和SLM试件均大于65°为疏水性材料,并不是细胞粘附的最佳接触角度。扫描电镜结果提示,EBM与SLM表面形态相似,但不是最佳利于细胞粘附的表面形态。成分分析结果表明：三种试件中非金属元素C、H、O、N的含量均在正常范围内,三种试件表面成分均为α-Ti,且SLM和EBM表面均可形成氧化膜。没有观察到金属成分偏析的现象。显微硬度结果表明：三种试件硬度差别不是很明显。EBM硬度最高,与SLM及锻造试件有统计学差异(P0.05),SLM及锻造试件之间无统计学差异(P0.05)。电化学腐蚀实验结果表明：EBM试件的热力学稳定性劣于其他两种试件。在电极电位1200mV时,SLM试件的耐腐蚀性最强；在电极电位1200 mV时,EBM试件的耐腐性最强。浸泡实验结果表明,SLM试件的耐腐蚀性最强。培养液金属离子析出浓度表明：SLM试件Al、V离子的析出量最少,与电化学腐蚀实验结果相吻合。但三种试件析出Al、V离子的含量均为微克级,不足以对细胞的粘附、增殖造成影响。生物相容性：细胞计数及扫描电镜结果表明：BMSC在三种试件上的粘附、增殖能力相近,随着培养时间的延长,细胞数量增加明显,且细胞形态变化明显。透射电镜结果显示：BMSC及比格犬肝、肾组织超微结构与锻造件及正常肝肾组织无明显差别,没有发现受损伤的迹象。组织学及大体观察结果显示：试件被一层纤维组织囊所包绕,未发现炎性组织及金属颗粒。单细胞电泳实验结果表明：未发现比格犬肝肾组织DNA损伤。[结论]EBM与SLM工艺打印的钛合金试件具有良好的理化性能和生物相容性,均适合应用到体内,但有必要根据具体应用部位对其性能加以调整及改进。
[Abstract]:[Objective] to compare the physical and chemical properties and biocompatibility of Ti-6A1-4V specimens made by electron beam selective melting (EBM) and laser selective melting (SLM), and to provide theoretical basis for the clinical application of 3D printing titanium alloys: the application of electron beam selective melting (EBM) and laser selective melting (SLM) to prepare Ti-6A1-4V Alloy specimens were used as control. (1) microstructures were observed by optical microscopy, scanning electron microscopy, transmission electron microscopy and EBSD methods; (2) the composition analysis was carried out by XRD, EDS, XPS and GB/T4698 series methods; (3) the hydrophilicity of EBM and SLM specimens was detected by contact angle test method; (4) three kinds of Vivtorinox hardness methods were used to detect three species. Vivtorinox hardness of test parts. (5) use roughness meter to detect the surface roughness of EBM and SLM specimens; (6) electrochemical experiment, soaking experiment, and cell culture liquid ion precipitation test method to detect its corrosion resistance. Biocompatibility: in vitro study for EBM, SLM and forging three. In vivo research for EBM and normal tissue. (1) application of scanning electricity The method of microscope and cell count was used to observe the adherence and proliferation of bone marrow stromal stem cells (BMSC) at different time points. (2) the application of transmission electron microscopy to observe the BMSC on the different craft specimens and the liver of beagle dog after 52 weeks of subcutaneous implantation and the damage of the ultrastructure of renal tissue. (3) application Histological staining and gross observation were used to observe the abnormality of the tissue around Ti-6A1-4V specimens. (4) a single cell electrophoresis test (comet experiment) was used to detect the liver of beagle dogs after 52 weeks of subcutaneous implantation and whether the renal tissue was damaged. [results] physical and chemical properties: the microscopic structure of the three specimens showed that the microstructure of the three specimens was not. EBM and SLM are martensitic tissues, and most of SLM are Martensitic, and most of the SLM grains are smaller than EBM. Many short dislocations and twins are found in SLM specimens. The precipitation of intermetallic compounds is found in EBM specimens. The surface roughness results show that the surface roughness of EBM and SLM is beneficial to cell adhesion. Contact angle experiment The results showed that both EBM and SLM specimens were more than 65 degrees as hydrophobic material and not the best contact angle of cell adhesion. The results of scanning electron microscopy showed that the surface morphology of EBM and SLM was similar, but not the best surface morphology for cell adhesion. The results of component analysis showed that the content of the non-metallic elements of the three specimens, C, H, O, and N, were in the normal range. The surface composition of the three specimens were all alpha -Ti, and the surface of SLM and EBM could form an oxide film. The phenomenon of metal segregation was not observed. The microhardness results showed that the hardness difference between the three specimens was not very obvious, and the hardness of.EBM was the highest, and there was statistical difference between the SLM and the forging specimens (P0.05), and there was no statistical difference between the SLM and the forging specimens (P0.). 05). The results of electrochemical corrosion test show that the thermodynamic stability of the EBM specimen is worse than the other two kinds. The corrosion resistance of the SLM specimen is the strongest when the electrode potential is 1200mV; the corrosion resistance of the EBM specimen is the strongest when the electrode potential is 1200 mV. The results of soaking experiments show that the corrosion resistance of the SLM specimen is the strongest. Ming: SLM sample Al, V ion precipitation of the least, and electrochemical corrosion experimental results coincide. But the three specimens precipitated Al, V ion content is microgram level, not enough to cell adhesion, proliferation effect. Biocompatibility: cell count and scanning electron microscope results show that BMSC on the three specimens adhered to the proliferation ability is similar. With the prolongation of the culture time, the number of cells increased obviously and the cell morphology changed obviously. The transmission electron microscope showed that the ultrastructure of BMSC and beagle liver, the renal tissue ultrastructure was not significantly different from the forged parts and normal liver and kidney tissues, and no signs of injury were found. Histology and gross observation showed that the specimen was covered with a layer of fibrous tissue sac. The results of single cell electrophoresis showed that no DNA damage was found in the hepatorenal tissues of the Beagle dogs. [conclusion the titanium alloys printed by]EBM and SLM have good physical and chemical properties and biocompatibility, and are suitable for application to the body, but it is necessary to adjust their performance according to the specific application sites. Whole and improvement.
【学位授予单位】：中国人民解放军医学院
【学位级别】：博士
【学位授予年份】：2016
【分类号】：R318.08

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