不同孔径分布多孔钛的力学性能

从生物学角度出发设计并制备2种不同孔径分布的多孔钛,并研究其力学性能。采用造孔剂烧结方法制备孔隙率为36%~63%的多孔钛,通过室温压缩测试其力学性能。多孔钛的弹性模量和抗压强度分别在2.662~18 GPa和94.05~468.57 MPa范围内,且都随着孔隙率的增加而降低。抗压强度和孔隙率的关系曲线呈现完全的线性特征,表明抗压强度主要受孔隙率的影响,几乎不受孔径的影响。Gibson-Ashby力学关系分析结果显示：常数项C值的差异说明孔径分布对多孔钛的屈服强度有一定的影响;密度指数n值均大于临界值3,表明这2种不同孔径的多孔钛的变形方式相同,为孔壁的屈曲作用。     

Structural and mechanical characteristics of porous 316L stainless steel fabricated by indirect selective laser sintering

Selective laser sintering (SLS) technique is capable of rapidly fabricating customized implants with porous structure. A simple encapsulation process was developed to coat 316L stainless steel (316L SS) powder with ethylene-vinyl acetate copolymer (EVA). Subsequently, porous 316L SS was prepared by SLS preforming of EVA-coated metal powders, debinding and sintering in hydrogen atmosphere. The effects of processing parameters on pore characteristics and mechanical properties were analyzed. The results indicate that the porosity of green body mainly depends on laser energy density, while the pore features and mechanical properties of sintered specimens are largely dominated by sintering temperature. After sintering at 1100–1300 °C, the average pore size and porosity are 160–35 μm and 58–28%, respectively. In addition, the elastic modulus and compressive yield strength are 1.58–6.64 GPa and 15.5–52.8 MPa, respectively. It is revealed that the pore structural parameters and mechanical properties of the as-sintered porous 316L SS can be controlled readily to match with those of cancellous bone by modification of SLS processing parameters and subsequent sintering temperature.     

Fabrication of Bioceramic Bone Scaffolds for Tissue Engineering

In this study, microhydroxyapatite and nanosilica sol were used as the raw materials for fabrication of bioceramic bone scaffold using selective laser sintering technology in a self-developed 3D Printing apparatus. When the fluidity of ceramic slurry is matched with suitable laser processing parameters, a controlled pore size of porous bone scaffold can be fabricated under a lower laser energy. Results shown that the fabricated scaffolds have a bending strength of 14.1 MPa, a compressive strength of 24 MPa, a surface roughness of 725 nm, a pore size of 750 μm, an apparent porosity of 32%, and a optical density of 1.8. Results indicate that the mechanical strength of the scaffold can be improved after heat treatment at 1200 °C for 2 h, while simultaneously increasing surface roughness conducive to osteoprogenitor cell adhesion. MTT method and SEM observations confirmed that bone scaffolds fabricated under the optimal manufacturing process possess suitable biocompatibility and mechanical properties, allowing smooth adhesion and proliferation of osteoblast-like cells. Therefore, they have great potential for development in the field of tissue engineering.     

SLM制备径向梯度多孔钛/钽及其表征研究

利用增材制造技术制作仿天然骨的径向梯度多孔钛/钽骨科植入物具有广阔的前景。基于三周期极小曲面（triply minimal surfaces,TPMS）建模法建立了平均孔隙率为70%的圆柱型径向梯度孔隙结构,孔隙率由中轴线（90%）向圆周面（30%）逐渐降低。利用激光选区熔化(Selected Laser Melting, SLM)工艺制作径向梯度多孔钛/钽。光学显微镜,扫描电镜,Micro-CT检测结果共同显示,SLM径向梯度多孔钛/钽的孔隙结构与设计特征一致。SLM工艺制作的径向梯度多孔钛/钽的孔隙率分别为73.18%与68.18%。力学测试结果表明,梯度多孔钛/钽的弹性模量分别为3.96±0.19GPa与3.47±0.25GPa,抗压强度分别为90.83±3.35MPa与93.27±1.24MPa。梯度多孔钛/钽的弹性模量与抗压强度分别显著高于均匀多孔钛/钽（孔隙率为70.11%的均匀多孔钛弹性模量为2.34±0.48GPa,抗压强度为67.63±1.33MPa,孔隙率为65.39%的均匀多孔钽弹性模量为1.69±0.49GPa,抗压强度为68.56±0.41MPa）。体外细胞相容性实验证明,径向梯度多孔钛/钽均具有良好的生物相容性,适合间充质干细胞与肌肉细胞的粘附生长。SLM工艺制作的径向梯度多孔钛/钽比均匀多孔钛/钽具有与天然骨组织更相近的结构与性能,是理想的骨缺损修复替代物。     

Nanospike surface-modified bionic porous titanium implant and in vitro osteogenic performance

This work aimed to prepare the nanospike surface-modified bionic porous titanium implants that feature favorable osteointegration performance and anti-bacterial functions. The implant was prepared using freeze casting, and nanospike surface-modification of the implant was performed using thermal oxidation. The pore morphology and size, mechanical properties, and osteogenic performance of the implants were analyzed and discussed. The results showed that when the volume ratio of titanium powder in slurry was set to be 10%, the porosity, pore diameter, compressive strength, and elastic modulus of the porous samples were (58.32±1.08)%, (126.17±18.64) μm, (58.51±20.38) MPa and (1.70±0.52) GPa, respectively. When the porous sample was sintered at a temperature of 1200 °C for 1 h, these values were (58.24±1.50)%, (124.16±13.64) μm, (54.77±27.55) MPa and (1.63±0.30) GPa, respectively. The nanospike surface-modified bionic porous titanium implants had favorable pore morphology and size, mechanical properties and osteointegration performance through technology optimization, and showed significant clinical application prospect.     

Preparation of porous Ta-10%Nb alloy scaffold and its in vitro biocompatibility evaluation using MC3T3-E1 cells

A highly porous Ta-10%Nb alloy was successfully prepared for tissue engineering via the methods of the sponge impregnation and sintering techniques. The porous Ta-10%Nb alloy offers the capability of processing a pore size of 300-600 μm, a porosity of (68.0±0.41)%, and open porosity of (93.5±2.6)%. The alloy also shows desirable mechanical properties similar to those of cancellous bone with the elastic modulus and the comprehensive strength of (2.54±0.5) GPa and (83.43±2.5) MPa, respectively. The morphology of the pores in the porous Ta-Nb alloy shows a good interconnected three-dimension (3D) network open cell structure. It is also found that the rat MC3T3-E1 cell can well adhere, grow and proliferate on the porous Ta-Nb alloy. The interaction of the porous alloy on cells is attributed to its desirable pore structure, porosity and the great surface area. The advanced mechanical and biocompatible properties of the porous alloy indicate that this material has promising potential applications in tissue engineering.     

Fabrication of Entangled Tough Titanium Wires Materials and Influence on Three-Dimensional Structure and Properties

Pure titanium (Ti) TA1 fibers/wires with 0.08 and 0.15 mm diameters were processed by a novel method that combined press forming, vacuum sintering (≥10^?2 Pa), and heat treatment to fabricate entangled Ti wire materials (ETWMs). The ETWMs exhibited a total porosity ranging from 44.2 ± 0.1 to 81.2 ± 0.1% and an open porosity ranging from 43.5 ± 0.1 to 80.9 ± 0.1%. The processing parameters of fiber diameter, formation pressure, sintering temperature, and sintering time were applied to examine porous ETWM morphology, porosity, pore size, and mechanical properties. The importance of primary factors controlling porous structure and porosity in ETWMs were found to be fiber/wire diameter > formation pressure > sintering temperature > sintering time. Furthermore, Ti fiber diameter was shown to directly impact pore size. High formation pressure resulted in a fine, uniform porous structure with low porosity. Sintering at high temperature for long-time periods promoted sintering point formation, resulting in neck coarsening. This effect contributed to the characteristic mechanical properties observed in these ETWMs. If the sintering effect is considered in isolation, ETWMs fabricated with 0.08 mm diameter Ti fibers/wires and sintered at 1300 °C for 90 min achieved smaller, more uniform porous structures that further exhibited improved connections among fibers/wires and excellent mechanical properties.     

Fabrication of lotus-type porous Mg−Mn alloys by metal/gas eutectic unidirectional solidification

Lotus-type porous Mg–xMn (x=0, 1, 2 and 3 wt.%) alloys were fabricated by metal/gas eutectic unidirectional solidification (the Gasar process). The effects of Mn addition and the fabrication process on the porosity, pore diameter and microstructure of the porous Mg−Mn alloy were investigated. Mn addition improved the Mn precipitates and increased the porosity and pore diameter. With increasing hydrogen pressure from 0.1 to 0.6 MPa, the overall porosity of the Mg−2wt.%Mn ingot decreased from 55.3% to 38.4%, and the average pore diameter also decreased from 2465 to 312 μm. Based on a theoretical model of the change in the porosity with the hydrogen pressure, the calculated results were in good agreement with the experimental results. It is shown that this technique is a promising method to fabricate Gasar Mg–Mn alloys with uniform and controllable pore structure.     

多孔CoCrNi中熵合金的制备和吸能特性分析

本文采用粉末烧结-溶解法成功制备了孔隙率为63%~78%,孔径1.3~2.2mm的多孔CoCrNi中熵合金,借助SEM和XRD对试样的孔形貌和物相组成进行分析,并对试样进行轴向准静态压缩实验研究。结果表明：多孔CoCrNi中熵合金的弹性模量和屈服平台应力均随孔隙率、孔径的增大而减小;相对孔隙率而言,孔径对力学性能的影响程度较低;不同孔隙率的多孔CoCrNi中熵合金其致密应变下单位体积的能量吸收值为34.8~14.3MJ/m₃^,约为泡沫铝的3.8倍,且5种孔隙率的理想吸能效率(I)都接近0.8,说明该多孔CoCrNi中熵合金有潜力成为一种理想的吸能材料。     

Microstructure,Mechanical Properties and Corrosion Behavior of Porous Mg-6 wt.% Zn Scaffolds for Bone Tissue Engineering

Porous Mg-based scaffolds have been extensively researched as biodegradable implants due to their attractive biological and excellent mechanical properties. In this study, porous Mg-6 wt.% Zn scaffolds were prepared by powder metallurgy using ammonium bicarbonate particles as space-holder particles. The effects of space-holder particle content on the microstructure, mechanical properties and corrosion resistance of the Mg-6 wt.% Zn scaffolds were studied. The mean porosity and pore size of the open-cellular scaffolds were within the range 6.7-52.2% and 32.3-384.2 µm, respectively. Slight oxidation was observed at the grain boundaries and on the pore walls. The Mg-6 wt.% Zn scaffolds were shown to possess mechanical properties comparable with those of natural bone and had variable in vitro degradation rates. Increased content of space-holder particles negatively affected the mechanical behavior and corrosion resistance of the Mg-6 wt.% Zn scaffolds, especially when higher than 20%. These results suggest that porous Mg-6 wt.% Zn scaffolds are promising materials for application in bone tissue engineering.     

Influence of Hot Isostatic Pressing on the Microstructure and Mechanical Properties of a Spray-Formed Al-4.5 wt.% Cu Alloy

Al-4.5 wt.% Cu alloy was spray atomized and deposited at varied spray heights ranging from 300 to 390 mm. The average grain sizes decreased from ~ 29 to ~ 18 μm and a concomitant increase in the hardness and the 0.2% yield strength (YS) with increase in the spray height. The respective hardness values of SF-300, SF-340, and SF-390 are 451 ± 59, 530 ± 39, and 726 ± 39 MPa and the YS are 108 ± 7, 115 ± 8, and 159 ± 10 MPa. The transmission electron micrographs revealed the morphological changes of the Al₂Cu phase from irregular shaped to small plate-shaped and then subsequently to spheroidal shape due to high undercooling encountered during spray atomization with increase in spray height from 300 to 390 mm. The porosity of the spray formed deposits varied between 5 to 12%. Hot isostatic pressing of spray deposits reduced the porosity to less than 0.5% without any appreciable increase in grain size. A dislocation creep mechanism seems to be operative during the secondary processing. A comparison between as-spray formed and hot isostatically pressed deposits exemplifies improvement in mechanical properties as a result of elimination of porosity without affecting the fine grain sizes achieved during the spray-forming process.     

Processing and characterization of porous Ti2AlC with controlled porosity and pore size

In this work, we demonstrate a simple and inexpensive way to fabricate porous Ti₂AlC, one of the best studied materials from the MAX phase family, with controlled porosity and pore size. This was achieved by using NaCl as the pore former, which was dissolved after cold pressing but before pressureless sintering at 1400 °C. Porous Ti₂AlC with samples a volume fraction of porosity ranging from ～10 to ～71 vol.% and different pore size ranges, i.e. 42–83, 77–276 and 167–545 μm, were successfully fabricated. Fabricated samples were systematically characterized to determine their phase composition, morphology and porosity. Room temperature elastic moduli, compressive strength and thermal conductivity were determined as a function of porosity and/or pore size. For comparison, several samples pressureless-sintered without NaCl pore former, or fabricated by spark plasma sintering, were also characterized. The effects of porosity and/or pore size on the room temperature elastic moduli, compressive strength and thermal conductivity of porous Ti₂AlC are reported and discussed in this work. It follows that porosity can be a useful microstructural parameter to tune mechanical and thermal properties of Ti₂AlC.     

Gasar工艺下藕状多孔银的气孔结构研究

金属-气体共晶定向凝固（Gasar)是制备藕状多孔金属的新工艺,利用自行研制的Gasar装置,成功地制备了不同纯氧分压下的藕状多孔银试样,研究了氧气分压对藕状多孔银气孔形貌（气孔率、气孔尺寸和分布、气泡形核）的影响。结果表明：氧气分压对气孔形貌影响十分显著。随着氧气压力的增加,气孔率增大而平均气孔直径减小。     

Highly Porous NiTi with Isotropic Pore Morphology Fabricated by Self-Propagated High-Temperature Synthesis

Highly porous NiTi with isotropic pore morphology has been successfully produced by self-propagating high-temperature synthesis of elemental Ni/Ti metallic powders. The effects of adding urea and NaCl as temporary pore fillers were investigated on pore morphology, microstructure, chemical composition, and the phase transformation temperatures of specimens. These parameters were studied by optical microscopy, scanning electron microscopy, x-ray diffraction, and differential scanning calorimetry (DSC). Highly porous specimens were obtained with up to 83% total porosity and pore sizes between 300 and 500 μm in diameter. Results show pore characteristics were improved from anisotropic to isotropic and pore morphology was changed from channel-like to irregular by adding pore filler powders. Furthermore, the highly porous specimens produced when using urea as a space holder, were of more uniform composition in comparison to NaCl. DSC results showed that a two-step martensitic phase transformation takes place during the cooling cycles and the austenite finish temperature (A _f) is close to human body temperature. Compression test results reveal that the compressive strength of highly porous NiTi is about 155 MPa and recoverable strain about 6% in superelasticity regime.     

Effects of porosity on tensile mechanical properties of porous FeAl intermetallics

Uniaxial tensile tests and scanning electron microscopy (SEM) experiments were carried out on the porous FeAl intermetallics (porosities of 41.1%, 44.2% and 49.3%, pore size of 15–30 μm) prepared by our research group to study the macroscopic mechanical properties and microscopic failure mechanism. The results show that the tensile σ–ɛ curves of the porous FeAl with different porosities can be divided into four stages: elasticity, yielding, strengthening and failure, without necking phenomenon. The elastic modulus, ultimate strength and elongation decrease with the increase of porosity and the elongation is much lower than 5%. A macroscopic brittle fracture appears, and the microscopic fracture mechanism is mainly intergranular fracture, depending on the Al content in the dense FeAl intermetallics. In addition, the stochastic porous model (SPM) with random pore structure size and distribution is established by designing a self-compiling generation program in FORTRAN language. Combined with the secondary development platform of finite element software ANSYS, the effective elastic moduli of the porous FeAl can be determined by elastic analysis of SPM and they are close to the experimental values, which can verify the validity of the established SPM for analyzing the elastic properties of the porous material.     

Rapid fabrication of function-structure-integrated NiTi alloys: Towards a combination of excellent superelasticity and favorable bioactivity

Porous NiTi has brought new expectations to the field of orthopaedic implants due to its excellent mechanical properties such as high strength and superelasticity together with good biocompatibility. In order to facilitate the surrounding bone tissue ingrowth into the implanted porous alloy, reasonably large sized pores and a high amount of porosity are required. There is, however, a major challenge for clinical applications: the higher the porosity, the worse are the mechanical properties and the superelasticity. In this work, therefore, function-structure-integrated NiTi alloys consisting of a central solid and an outer porous layer were fabricated by spark plasma sintering (SPS). When sintered at 750 °C, the NiTi alloy with 14% porosity in the inner part and 49% porosity as well as 350 μm average pore size in the outer layer exhibits an exceptionally high compressive strength (∼1375 MPa), together with an excellent superelastic recovery strain (>4%) and favorable cellular affinity (ROS1728 osteoblasts). Altogether, this work provides a strategy to design materials with function-structure integration and suggests that properly designed function-structure integrated NiTi alloys may be promising as advanced bone implants.     

冷冻-凝胶成形法制备定向通孔氧化铝陶瓷

由叔丁醇、氧化铝、丙烯酰胺组成的20%(体积分数,下同)陶瓷浆料,在温度梯度的诱导下,用冷冻-凝胶成形法制备了具有定向通孔结构的氧化铝陶瓷坯体.经过烧结后,制备出了高孔隙率、高强度的定向通孔陶瓷,50%气孔率的陶瓷体具有110 MPa的轴向压缩强度.还研究了距离冷端不同位置孔隙的孔径、开孔率变化规律.     

A Comparative Study on the Mechanical Behavior of Porous Titanium and NiTi Produced by a Space Holder Technique

NiTi and Ti porous specimens with appropriate pore characteristics for biomedical applications are produced by space holder method. Porosities of the specimens linearly increase from 14 to 65 and 42 to 70% for the Ti and NiTi specimens, respectively, with the urea space holder. Mechanical properties such as stiffness, fracture strain, and strength of the porous NiTi and Ti are adjustable with pore characteristics. The apparent elasticity modulus of NiTi specimens decrease from 3.5 to 0.73 GPa as porosity increases. Since the initial linear part of the stress-strain curve consists of elastic behavior, formation of stress-induced martensite, deformation and/or detwinning of martensite variants, and plastic deformation, the unloading slope of stress-strain curves is a better approximation for the elasticity modulus of the NiTi porous specimens as it is proved by an isotropic cubic cell model. The unloading slope of the NiTi specimen with 61% porosity is 3.1 GPa, while the apparent elasticity or loading slope is 0.85 GPa. In comparison to Ti, the high, recoverable strain of NiTi improves capability of it as a good candidate for bone replacement. Moreover, in contrast to Ti specimens, hysteresis loops are clearly observed in the stress-strain curves of NiTi specimens.     

Pore formation mechanism and characterization of porous NiTi shape memory alloys synthesized by capsule-free hot isostatic pressing

Porous NiTi alloys with different porosities were fabricated by capsule-free hot isostatic pressing (CF-HIP) with ammonium acid carbonate (NH₄HCO₃) as a space-holder. The microstructure and porosity of porous NiTi produced with different NH₄HCO₃ contents and sintering temperatures were determined. Two different creep expansion models are used to explain the pore expansion mechanism during the sintering process, which involves slow and continuous reduction of the argon pressure at high temperatures. When the NH₄HCO₃ content is 30 wt.% and the sintering temperature is 1050 °C, an ideal porous NiTi alloy with 48 vol.% porosity and circular pores (50–800 μm) is obtained. Compression tests indicate that the porous NiTi alloys with 21–48% porosity possess not only lower Young’s moduli of 6–11 GPa (close to that of human bones) but also higher compression strength and excellent superelasticity. Cell cultures reveal that the porous NiTi prepared here has no apparent cytotoxicity. The porous materials are thus promising biomaterials in hard tissue replacements.     

多孔金属结合剂CBN砂轮孔隙结构对磨料层胎体力学性能的影响

为解决多孔金属结合剂CBN砂轮在高孔隙率下的强度下降问题,采用球形尿素颗粒为造孔剂,制作孔径、孔形和孔隙可控的多孔金属结合剂砂轮磨料层胎体,研究不同载荷情况下的孔隙率和孔隙排布等孔隙结构因素,对多孔金属结合剂磨料层胎体力学性能的影响规律。结果表明:孔隙有序排布时的胎体弹性模量要小于孔隙无序排布的;胎体材料的屈服强度随孔隙率增大而下降;在相同孔隙率下,孔隙有序排布的胎体,在纵向受压、孔隙正向排布的情况下屈服强度更高。