Optimization on hydrogenation-dehydrogenation preparation of titanium powders by SHS
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摘要: 为优化自蔓延高温合成法氢化脱氢制备钛粉工艺过程，改变传统钢球球磨为闭环气流研磨，改变传统抽空脱氢工艺为减压点燃工艺，研究了优化工艺下自蔓延高温合成法氢化和脱氢前后样品微观结构、物相组成、化学成分和粒度分布。结果表明，自蔓延高温合成氢化制得的氢化钛氢含量较高（4.662%，质量分数），闭环气流研磨氢化后样品粒度均匀，粒度分布范围为40～250 μm。与传统抽空脱氢工艺相比，减压点燃脱氢工艺有助于控制钛粉样品中N、O、C含量。Abstract: To optimize the hydrogenation-dehydrogenation process for preparing titanium powders by self-propagating high-temperature synthesis (SHS) method, the traditional steel ball milling process was replaced by the new closed-loop air current grinding process, and the traditional evacuation process for dehydrogenation process was replaced by the decompression-ignition process. The microstructure, phase component, chemical composition, and particle size distribution of the samples prepared by the optimization process were studied. In the results, the hydrogen mass fraction in the titanium hydride samples is high (4.662%) after SHS hydrogenation, and the particle size distribution of the TiH2 particles is uniform with the range of 40~250 μm after the closed-loop air flow grinding process. The new dehydrogenation process is beneficial to control the N, O, and C content in the titanium powder samples.
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图 1 自蔓延高温合成技术脱氢炉示意图（a）和物相及结构变化（b）
Figure 1. Schematic diagram of the dehydrogenation furnace used in HDH technology (a) and the variation of phase and structure (b)
图 3 氢化前原料海绵钛X射线衍射分析（a）、扫描电镜观察（（b）～（c））和能谱分析（（d）～（e））
Figure 3. XRD patterns (a), FESEM images ((b)~(c)), and EDS analysis ((d)~(e)) of the sponge titanium samples before hydrogenation
图 4 氢化试样X射线衍射分析（a）、吸氢前后海绵钛显微形貌（（b）～（c））和氢化试样元素分布能谱分析（（d）～（f））
Figure 4. XRD patterns of the hydrogenation samples (a), FESEM images of the sponge titanium samples before and after hydrogenation ((b)~(c)), and EDS analysis ((d)~(f)) of the hydrogenation samples after
图 5 自蔓延高温合成技术脱氢工艺
Figure 5. Dehydrogenation process of the TiH2 powders by HDH method;
图 6 脱氢试样X射线衍射分析（a）、扫描电镜观察（（b）～（c））和Ti元素分布能谱分析（（d）～（f））
Figure 6. XRD patterns (a), FESEM images ((b)~(c)), and Ti element distribution in EDS analysis ((d)~(f)) of the dehydrogenation samples
图 7 脱氢前后样品的粒度分布曲线
Figure 7. Particle size distribution curve of the sample before and after dehydrogenation
表 1 试样化学成分（质量分数）
Table 1. Chemical composition of samples
% 样品及状态 Si Fe Cl C N O Mn Mg H Sn Ni Cr Al Cu 海绵钛原料 0.005 0.017 0.040 0.006 0.003 0.051 0.001 0.005 0.001 0.004 0.001 0.002 0.003 0.005 氢化后氢化钛粉末 0.004 0.016 0.050 0.008 0.004 0.062 0.001 0.004 4.662 0.003 0.001 0.004 0.002 0.004 气流磨后氢化钛粉末 0.004 0.018 0.050 0.008 0.008 0.071 0.001 0.003 4.654 0.003 0.001 0.006 0.002 0.004 脱氢后钛粉 0.001 0.024 0.030 0.003 0.006 0.072 0.001 0.005 0.035 0.002 0.002 0.008 0.003 0.004 
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