Preparation of porous magnesium bulk as bone substitute implant by spark plasma sintering using sublimate material as pore-forming agent
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摘要: 以萘为造孔剂, 采用放电等离子烧结技术(spark plasma sintering, SPS)制备多孔镁块体材料。结果表明, 采用放电等离子烧结技术在470℃时可以制备出结构与尺寸可控性好、开孔率与孔隙率(44.25%)较高、粉体颗粒无明显长大的多孔金属镁块体材料。升华性造孔剂可对孔隙体积进行有效调节, 实现多孔镁材料体内小孔与大孔的合理搭配, 进一步改善多孔镁材料孔隙之间的连通性。将升华性造孔剂与放电等离子烧结技术相结合后, 对于开孔性与颗粒连接性要求较高的多孔金属材料制备具有技术优势, 并对解决传统造孔剂法制备生物多孔金属材料所面临的二次污染问题具有很好的借鉴意义。Abstract: The porous magnesium bulk as bone substitute implant was prepared by spark plasma sintering (SPS) using the sublimate material (naphthalene) as pore-forming agent. The results show that, the porous magnesium bulk in the controllable structure and size with higher porosity (44.25%) and non-obvious powder particle growth can be manufactured by spark plasma sintering at 470 ℃. The sublimation pore-forming agent can effectively adjust pore volume, realize the reasonable collocation between macropores and micropores, and improve pore connectivity in porous magnesium bulk. The secondary pollution problem resulted from the traditional method can be solved by the combination of sublimation pore-forming agent and spark plasma sintering technology, which is technical advantageous to prepare the porous metal material in high demand of porosity and particle connectivity.
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Key words:
- spark plasma sintering /
- sublimate material /
- pore-forming agent /
- porous magnesium bulk /
- porosity
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图 1 骨组织在多孔镁中生长示意图: (a)传统放电等离子烧结法制备多孔镁的孔隙构成; (b)满足人体植入用骨替代材料要求的多孔镁孔隙构成
Figure 1. Schematic diagram of pore structures of porous Mg bulk in bone tissue: (a) pore structures in porous Mg bulk prepared by traditional SPS; (b) pore structures in porous Mg bulk satisfied the requirements of bone tissue for human implant
图 2 原料颗粒的扫描电子显微形貌(a)镁粉; (b)萘粉
Figure 2. Scanning electron microscope (SEM) images of Mg powders (a) and naphthalene powders (b)
图 4 不同温度放电等离子烧结后多孔镁内部显微结构: (a) 380℃; (b) 410℃; (c) 440℃; (d) 470℃; (e) 510℃
Figure 4. SEM images of porous Mg bulks at different sintering temperatures: (a) 380℃; (b) 410℃; (c) 440℃; (d) 470℃; (e) 510℃
图 5 添加不同质量分数造孔剂烧结后多孔镁内部结构: (a) 0%; (b) 10%; (c) 15%; (d) 20%; (e) 25%
Figure 5. SEM images of porous Mg bulks added by pore-forming agent (naphthaline) in different mass fractions at 470℃: (a) without pore-forming agent; (b) 10%; (c) 15%; (d) 20%; (e) 25%
图 6 添加萘做造孔剂后多孔镁材料的X射线衍射图谱
Figure 6. X-ray diffraction patterns of porous Mg bulk added by pore-forming agent (naphthaline)
表 1 不同温度放电等离子烧结后多孔镁材料的物理性能
Table 1. Physical properties of porous Mg bulk sintered at different temperatures
样品编号 烧结温度/ ℃ 抗压强度/ MPa 样品质量/ g 多孔镁尺寸/ mm 密度/ (g·cm-3) 孔隙率/ % 直径 高度 松装镁粉 ― ― 4.34 15.50 20.00 1.15 33.87 # a 380 0.075 4.29 15.48 19.97 1.16 33.33 # b 410 0.212 4.25 15.45 19.23 1.18 32.18 # c 440 0.821 4.23 15.33 19.10 1.20 31.03 # d 470 1.502 4.18 15.21 18.71 1.23 29.31 # e 510 2.879 4.09 13.12 14.29 1.39 20.11 
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表 2 添加不同质量分数造孔剂烧结后多孔镁材料的物理性能
Table 2. Physical properties of porous Mg bulk added by pore-forming agent (naphthaline) in different mass fractions at 470℃
样品编号 造孔剂质量分数/ % 抗压强度/ MPa 样品质量/ g 多孔镁尺寸/ mm 密度/ (g·cm-3) 孔隙率/ % 直径 高度 松装镁粉 0 ― 4.34 15.50 20.00 1.15 33.87 # a 0 1.50 4.18 15.21 18.71 1.23 29.31 # b 5 1.44 4.01 15.48 18.77 1.14 34.48 # c 10 1.26 3.86 15.47 18.55 1.11 36.02 # d 15 1.17 3.54 15.47 18.40 1.03 40.80 # e 20 1.02 3.32 15.47 18.21 0.97 44.25 # f 25 0.42 3.11 15.47 18.03 0.91 47.70
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