Porous titanium prepared by metal injection molding based on space-holder technique
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摘要: 以聚甲基丙烯酸甲酯（PMMA）为造孔剂，聚甲醛（POM）为主要粘结剂，通过金属注射成形和高真空烧结制备了多孔钛。研究了PMMA在金属注射成形中对多孔钛孔隙特征的影响及烧结温度对多孔钛孔隙特征的影响。结果表明，密炼过程中PMMA与POM等有机粘结剂混合在一起，失去其原有颗粒特征（粒径与形状）；热脱脂过程中PMMA集中在350～420 ℃区间先于高密度聚乙烯（HDPE）分解，起到造孔作用，但孔隙形状不可控且孔径远小于其原始颗粒尺寸；在1100～1250 ℃烧结区间内，提高烧结温度时多孔钛的开孔率与孔径均呈下降趋势，当烧结温度为1150～1200 ℃时，多孔钛开孔率为34%～35%，孔径为9.1 µm。Abstract: Porous titanium was prepared by metal injection molding (MIM) and high vacuum sintering using polymethyl methacrylate (PMMA) particles as pore forming agent and polyformaldehyde (POM) as main binder. The effects of PMMA and sintering temperature on the pore characteristics of porous titanium were investigated in detail. The results showed that PMMA particles are melted and mixed with organic binder together and lose their original particle characteristics (particle size and shape) during kneading. In the process of thermal debinding, PMMA decompose before high-density polyethylene (HDPE) in the temperature range of 350～420 ℃, which play the role of pore formation, but the shape of pores was irregular and the pore sizes are much smaller than the original PMMA particle sizes. In the sintering temperature range of 1100～1250 ℃, the opening porosity and pore sizes of porous titanium decrease with increasing of sintering temperature. When the sintering temperature is 1150～1200 ℃, the opening porosity of porous titanium is 34%～35%, and the pore size is about 9.1 μm.
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图 1 氢化脱氢钛粉与球形PMMA颗粒的微观形貌：(a)钛粉；(b) PMMA颗粒
Figure 1. SEM morphology of HDH titanium powder (a) and spherical PMMA particles (b)
图 2 注射生坯与喂料的密度
Figure 2. Densities of the injection molded green parts and the feedstock
图 3 注射生坯的断口微观组织：(a)二次电子图像；(b)背散射图像
Figure 3. Fracture morphology of the injection molded green part: (a) secondary electron image; (b) backscattered image
图 4 催化脱脂灰坯的断口微观组织
Figure 4. Fracture morphology of the degreased blank after catalytic debinding
图 6 HDPE、EVA和SA共混物的TG/DSC曲线
Figure 6. TG/DSC curve of the polymer blends HDPE, EVA and SA
图 8 脱脂灰坯中各高分子组分的质量分数及其热脱脂过程的失重率
Figure 8. Mass fraction and weight loss in thermal debinding of each polymer components in degreased blank
图 11 不同烧结温度制备的多孔钛的表面和内部（断口）微观组织：（a）、（e）1100 ℃；（b）、（f）1150 ℃；（c）、（g）1200 ℃；（d）、（h）1250 ℃
Figure 11. Surface morphologies (a~d) and internal porous features (e~h) of porous titanium sintered at different temperature: (a), (e) 1100 ℃; (b), (f) 1150 ℃; (c), (g) 1200 ℃; (d), (h) 1250 ℃
图 12 不同烧结温度制备的多孔钛的孔径分布曲线
Figure 12. Pore size distribution curve of porous titanium sintered at different temperatures
组分 熔融温度 / ℃ 热分解温度 / ℃ POM 175～180 280 HDPE 139 410～550 EVA 99 230 SA 150～176 350～380 PMMA >160 >270 
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表 2 不同烧结温度制备的多孔钛的孔隙特性
Table 2. Pore properties of porous titanium at different sintering temperatures
烧结温度 / ℃ 开孔率 / % 孔隙容积 / (mL·g−1) 比表面积 / (m2·g−1) 平均孔径 / μm 1100 40.08 0.1519 0.067 9.117 1150 35.57 0.1221 0.054 9.073 1200 34.70 0.1170 0.051 9.183 1250 26.69 0.0799 0.038 8.465
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