The microstructure evolution of nanohydroxapatite powder sintered for bone tissue engineering

Nanotechnology has been widely used to overcome the brittleness of coarse ceramics. Laser sintering is an effective approach for the preparation of nanoceramics due to the laser properties such as high energy density and rapid heating. In this study, the nanohydroxypatite (HAP) was used to prepare for artificial bone scaffold using a home-made selective laser sintering (SLS) system. The microstructure and the properties of the sintered nanoHAP are tested with scanning electron microscopy, X-ray diffraction and Fourier transform infrared spectroscopy. We found that the shape of nanoHAP particle changes from long needle-like to spherical or ellipsoidal after sintering, and the HAP particles grow up until they merge together with the increasing temperature. The tendency of preferred orientation reduces and the degree of crystallinity increases with the growth of nanoHAP. HAP dehydroxylation occurs during sintering. HAP decomposes to tetracalcium phosphate and β-calcium phosphate when the sintering temperature is over 1354°C (the laser power is 8.75?W). Sintered nanoHAP maintains a high degree of crystalline and nanometre scale when the laser power is 7.50?W, spot radius 2?mm, sintering time 4?s and thickness of the layer is 0.2?mm. This study presented the optimised technology parameters for the preparation of nanoceramics with a novel SLS system and demonstrated that the nanoceramics with nanosize scale can be obtained by this system.     

Preparation of poly(3-hydroxybutyrate)/nano-hydroxyapatite composite scaffolds for bone tissue engineering

Poly(3-hydroxybutyrate)/nano-hydroxyapatite (PHB/nHA) composite scaffolds were fabricated via powder mixing, compression moulding, and particle leaching technique. The scaffolds had high porosity with interconnected porous architecture, a favorable structure for cell attachment and new bone tissue ingrowth. A homogeneous dispersion and a uniform distribution of HA nanoparticles in the polymer matrix were obtained. The scaffolds exhibited improved compressive modulus and compressive strength, which were all in the range of compressive modulus and compressive strength of cancellous bone. In addition, the use of toxic organic solvents was eliminated. Thus, the fabricated PHB/nHA composite scaffolds tend to be promising for application in bone tissue engineering.     

Effect of process parameters on residual stress in selective laser melting of AlSi10Mg

ABSTRACT

Residual stress is a key indicator for measuring complex additive components, and its control method has received extensive attention. In this study, the finite element simulation of selective laser melting of AlSi10Mg was performed. It is found that the opposite laser scanning strategy can reduce the final residual stress of the sample. The effect of preheating the substrate to control the residual stress within a certain temperature range is obvious, and the laser scanning speed has the greatest influence on the Z-direction residual stress of the sample. The results show that the sag phenomenon is easy to occur at the laser scanning starting position, and the formed layer is the maximum residual stress region at the junction with the substrate.     

Characterization of poly(3-hydroxybutyrate)/nano-hydroxyapatite composite scaffolds fabricated without the use of organic solvents for bone tissue engineering applications

Poly(3-hydroxybutyrate)/nano-hydroxyapatite (PHB/nHA) composite scaffolds were fabricated without the use of organic solvents at different mass fractions of HA nanoparticles. HA nanoparticles were homogeneously dispersed as primary particles in the polymer matrix of the scaffolds at 10 and 15 wt.% nHA content. Agglomeration of HA nanoparticles occurred when the nHA content of the scaffolds reached 20 wt.%. All the scaffolds had high porosities with interconnected porous structure and optimized pore size ranges. Mechanical properties of all the scaffolds were in the range of mechanical properties of cancellous bone. Scaffolds were biocompatible to MG-63 cells in the indirect method of cytotoxicity evaluation. Also, the morphology of the attached MG-63 cells in direct contact with the scaffolds indicated the appropriate cell-scaffold interaction. Thus, the PHB/nHA composite scaffolds investigated in this study tend to be favorable for bone tissue engineering applications.     

纳米二氧化硅增强尼龙12选择性激光烧结成形件

使用纳米二氧化硅增强尼龙12选择性激光烧结(SLS)成形件,通过溶剂沉淀法制备SLS用纳米二氧化硅/尼龙12复合粉末材料,研究了纳米二氧化硅对SLS成形件力学性能的影响,结果表明:纳米二氧化硅以纳米尺寸均匀分散在尼龙12基体中:复合粉末的粒径比纯尼龙12的粉末小,因而有利于提高烧结速率及成形件精度;复合粉末比尼龙12的粉末具有更高的热稳定性;复合粉末烧结件的拉伸强度、拉伸模量以及冲击强度比纯尼龙12烧结件分别提高了约20.9%、39.4%和9.5%,说明纳米二氧化硅对尼龙12 SLS成形件的增强效果显著.     

A review on powder-based additive manufacturing for tissue engineering: selective laser sintering and inkjet 3D printing

Abstract

Since most starting materials for tissue engineering are in powder form, using powder-based additive manufacturing methods is attractive and practical. The principal point of employing additive manufacturing (AM) systems is to fabricate parts with arbitrary geometrical complexity with relatively minimal tooling cost and time. Selective laser sintering (SLS) and inkjet 3D printing (3DP) are two powerful and versatile AM techniques which are applicable to powder-based material systems. Hence, the latest state of knowledge available on the use of AM powder-based techniques in tissue engineering and their effect on mechanical and biological properties of fabricated tissues and scaffolds must be updated. Determining the effective setup of parameters, developing improved biocompatible/bioactive materials, and improving the mechanical/biological properties of laser sintered and 3D printed tissues are the three main concerns which have been investigated in this article.     

A review on powder-based additive manufacturing for tissue engineering: selective laser sintering and inkjet 3D printing

Since most starting materials for tissue engineering are in powder form, using powder-based additive manufacturing methods is attractive and practical. The principal point of employing additive manufacturing (AM) systems is to fabricate parts with arbitrary geometrical complexity with relatively minimal tooling cost and time. Selective laser sintering (SLS) and inkjet 3D printing (3DP) are two powerful and versatile AM techniques which are applicable to powder-based material systems. Hence, the latest state of knowledge available on the use of AM powder-based techniques in tissue engineering and their effect on mechanical and biological properties of fabricated tissues and scaffolds must be updated. Determining the effective setup of parameters, developing improved biocompatible/bioactive materials, and improving the mechanical/biological properties of laser sintered and 3D printed tissues are the three main concerns which have been investigated in this article.     

Study on the reinforcement of nanosilica on the selective laser sintered nylon–12 parts

使用纳米二氧化硅增强尼龙12选择性激光烧结(SLS)成形件, 通过溶剂沉淀法制备SLS用纳米二氧化硅/尼龙12复合粉末材料, 研究了纳米二氧化硅对SLS成形件力学性能的影响. 结果表明: 纳米二氧化硅以纳米尺寸均匀分散在尼龙12基体中: 复合粉末的粒径比纯尼龙12的粉末小, 因而有利于提高烧结速率及成形件精度; 复合粉末比尼龙12的粉末具有更高的热稳定性; 复合粉末烧结件的拉伸强度、拉伸模量以及冲击强度比纯尼龙12烧结件分别提高了约20.9%、39.4%和9.5%, 说明纳米二氧化硅对尼龙12 SLS成形件的增强效果显著.     

尼龙12覆膜铝粉激光烧结成形件的性能研究

常用的机械混合法很难将尼龙12和金属粉末材料混合均匀,容易出现偏聚,因而会造成选择性激光烧结(SLS)成形件中存在局部强度弱点、翘曲等缺陷.为此,提出了通过溶液沉淀法制备SLS成形用尼龙12覆膜铝粉,利用扫描电镜观察了尼龙12覆膜铝粉及烧结件断口的微观形貌,研究了铝粉含量及粒径对SLS成形件性能的影响.结果表明:尼龙12均匀地包覆在铝粉表面,无裸露铝粉颗粒存在,表明成功制备得到了尼龙12覆膜铝粉材料;当铝粉含量从0增大到50%时,烧结件的热变形温度、拉伸强度、弯曲强度、弯曲模量及硬度比纯尼龙烧结件分别提高了87℃、10.4%、62.1%、122.3%及70.4%;烧结件的拉伸强度、断裂伸长率及冲击强度均随着铝粉平均粒径的减小而增大.     

Fabrication and characterization of chitosan microspheres agglomerated scaffolds for bone tissue engineering

In the presented paper authors describe a method for bone scaffolds fabrication. The technique is based on the agglomeration of chitosan microspheres. The fabrication process is complex and consists of a few steps: chitosan spheres extrusion, scaffold formation by compression followed by the spheres agglomeration and bonding with cross-linking agent (STPP, sodium tripolyphosphate). The described method allows manufacturing of porous materials with controllable shape, pore size distribution and their interconnectivity. In this technique 3D scaffold porosity can be regulated by altering spheres diameter. Authors studied influence of cross-linker concentrations and time of cross-linking process on the scaffold morphology, mechanical properties, enzymatic degradation rate (in the presence of lysozyme) and human osteoblasts response. Surface morphology and topography were evaluated by SEM. Porosity and pore interconnectivity were observed via μCT scanning. Mechanical tests showed that chitosan scaffolds perform compression characteristic (Young Modulus) similar to natural bone. Cytotoxicity established by XTT assay confirmed that most of the developed composite materials do not show toxic properties. Osteoblast adhesion and morphology were analyzed by SEM and optical microscopy.     

骨组织工程多孔支架材料性质及制备技术

多孔性生物可降解支架的选择和制备是组织工程技术成功运用的关键。从骨架的材料要求、常用的骨架材料、骨架的制备技术等几个方面对组织工程和生物降解支架的研究进行了综述 ,并对该研究的前景进行了展望     

Structure and properties of nano-hydroxypatite scaffolds for bone tissue engineering with a selective laser sintering system

In this study, nano-hydroxypatite (n-HAP) bone scaffolds are prepared by a homemade selective laser sintering (SLS) system based on rapid prototyping (RP) technology. The SLS system consists of a precise three-axis motion platform and a laser with its optical focusing device. The implementation of arbitrary complex movements based on the non-uniform rational B-Spline (NURBS) theory is realized in this system. The effects of the sintering processing parameters on the microstructure of n-HAP are tested with x-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy and scanning electron microscopy (SEM). The particles of n-HAP grow gradually and tend to become spherical-like from the initial needle-like shape, but still maintain a nanoscale structure at scanning speeds between 200 and 300 mm min(-1) when the laser power is 50 W, the light spot diameter 4 mm, and the layer thickness 0.3 mm. In addition, these changes do not result in decomposition of the n-HAP during the sintering process. The results suggest that the newly developed n-HAP scaffolds have the potential to serve as an excellent substrate in bone tissue engineering.     

聚乳酸组织工程支架表面涂覆钙磷盐的工艺研究

提出了以聚乳酸／钙磷盐／胶原的骨组织工程支架快速成形制造的材料系统，对比了两种在聚乳酸(PLA)表面涂覆钙磷盐的工艺．一种是将聚乳酸组织工程支架浸泡在模拟体液中采用平衡反应法沉积钙磷盐；另一种是在聚乳酸薄膜上采用非平衡反应法沉积钙磷盐；系统地研究了沉积时间和沉积量、钙磷摩尔比和相结构演变的关系；通过控制反应时间和调整反应物配比获得磷酸四钙(TetCP)-PLA和无定形磷酸钙(ACP)—PLA等材料组合；并对所获得的复合材料进行生物相容性试验．对比试验证明细胞在材料表面生长良好，采用两种方法涂覆钙磷盐均改进了聚乳酸的生物相容性．     

激光增材制造用SiC粉末制备及成形工艺探索

为制备高强度复杂形状SiC陶瓷零件,以酚醛树脂(PF)为粘接剂,分别采用机械混合法(SPM)和搅拌蒸发法(SPC)制备两种SiC复合粉末,并对两种粉末进行了SEM电镜扫描、SLS成形、碳化和渗硅反应烧结处理.研究表明,在激光功率10 W,分层厚度0.1 mm,扫描速2 000 mm/s,扫描间距0.2 mm时,SLS坯体密度大(1.259 g/cm3),生产效率高.利用SPC粉末制得的SLS坯体内部孔隙更多,碳化和渗硅烧结后坯体密度明显增加.采用SPC粉末所制零件最终力学性能更好,更适于生产.在最优工艺条件下,制备了复杂形状的高性能SiC零件.     

纤维素/聚醚砜共混物激光烧结弹性性能的分子动力学模拟

为提高选择性激光烧结(SLS)木塑复合粉末的成形件的力学强度,设计出可用于该项技术木塑复合粉末的新配方,制备了纤维素/聚醚砜(PES)和纤维素/聚丙烯(PP) 2种木塑复合粉末。利用分子力学和分子动力学模拟方法对纤维素/PES和纤维素/PP共混物进行共混计算,求得了纤维素分别与PES、PP的结合能分布曲线。通过建立不同质量比的纤维素/PES共混物分子模型,计算其Flory-Huggins相互作用参数和静态弹性性能,得到了纤维素含量对共混物弹性性能的影响;为验证模拟结果进行了纤维素/PES和纤维素/PP共混物的激光烧结实验。结果表明:相比较纤维素/PP复合粉末,纤维素与PES相容性更好,适用于选择性激光烧结技术;当纤维素加入质量分数为20%~25%时,材料的相容性达到最佳状态;所构建的纤维素/PES共混物模型可用于预测成形材料的弹性性能。      

Effect of different heat treatments on the microstructure and mechanical properties in selective laser melted INCONEL 718 alloy

The microstructure and tensile properties of selective laser melted (SLM) Inconel 718 alloy were studied in the as-printed and different heat treat conditions. The SLM as-print microstructures exhibited columnar grain structures with very fine dendritic structure with segregation of elements. Apart from the standard heat treatment, three other heat treat cycle variants were carried out in an attempt to remove the extensive segregation of elements and modify the textured grain structure of the SLM as-print microstructure. Increasing the homogenization temperature reduced the segregation and coarsened the grain structure. However, the grains still remained columnar, and the material became softer with reduction in strength. After the ageing treatment, the tensile strength improved significantly for all the heat treated samples, which is typical for precipitation hardening of IN718 alloy. The microstructures of the heat treated samples exhibited the needle shaped δ, carbides, and finely dispersed γ″, γ′ phases.     

The effect of laser energy input on the microstructure,physical and mechanical properties of Ti-6Al-4V alloys by selective laser melting

Selective laser melting is an advanced manufacturing process which can control the microstructure evolution and mechanical properties of as-manufactured products via various processing parameters. In this study, the porosity/relative density, surface quality, microstructure and mechanical properties were investigated on the selective laser melted Ti-6Al-4V alloy specimens fabricated with a wide range of laser energy inputs. It was found that the microstructure of selected laser melted Ti-6Al-4V alloys is typical of acicular martensites α′. Quantitative analysis reveals that the relative density, martensitic lath size and microhardness increase with the laser energy input. The surface quality is also substantially affected by the energy input.     

Effect of build direction on the fracture toughness and fatigue crack growth in selective laser melted Ti‐6Al‐4 V

Experimental investigation was conducted to evaluate the fracture toughness and fatigue crack growth characteristics in selective laser‐melted titanium 6Al‐4 V materials as a follow‐on to a previous study on high cycle fatigue. For both the fracture toughness and crack growth evaluation, the compact tension specimen geometry was used. It was found that the fracture toughness was lower than what would be expected from wrought or cast product forms in the same alloy. This was attributed to the rapidly cooled, martensitic microstructure, developed in the parts. At low stress ratios, the crack growth rates were faster than in wrought titanium but became comparable at higher ratios. The fracture toughness appears to be higher when the crack is oriented perpendicular to the build layers. The difference in the average threshold and critical stress intensity values for the crack growth results for the three orientations was within the scatter of the data, so there was essentially no difference. The same was true for the empirically derived Paris Law constants. Residual stresses were likely to have overshadowed any variation in crack growth because of microstructural directionalities associated with build orientation.     

A comprehensive study on variability of relative density in selective laser melting of Ti-6Al-4V

ABSTRACT

In this research, the effects of Selective Laser Melting (SLM) process parameters comprising laser power, scan speed, hatch space and scan pattern angle on the formation of porosity and subsequently density have been analysed. To improve the mechanical properties, post-processes (heat treatment) must be performed. Therefore, heat treatment was added to the design of experiment to analyse the effect of this process coupling with SLM process parameters on the value of density. A comprehensive design set with five levels for each parameter was selected so Taguchi L25 was used as the design of experiment. The significance of each parameter on obtained results was examined using statistical analysis (F-Test) and numerical model (interrogator analysis). The correlation between two process parameters was discussed by using 3D analytical and contour plots and the mechanisms behind these were discussed in depth. The contribution of this paper is a deep investigation of the relation of process parameters and heat treatment on density based on the Artificial Neural Network model. Results showed that better density is obtained with lower scan speed, laser power and scanning pattern angle. Meanwhile, for heat treatment and hatch space, the best density was obtained in their optimum range.     

烧结工艺对锶铁氧体永磁材料性能及结构的影响

研究了锶铁氧体烧结过程中烧结温度、恒温时间对锶铁氧体磁性能及结构的影响.结果表明,随烧结温度的升高,Br和(BH)max均增大,HCJ减小;随恒温时间的延长,变化趋势相同.优化试验结果为:烧结温度1180～1215 ℃,恒温时间2～3 h.