Effects of mechanical milling on microstructure and tensile properties of CoCrFeMnNi high-entropy alloys produced by spark plasma sintering
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摘要:
采用CoCrFeMnNi预合金粉末和放电等离子烧结工艺制备了全致密的粉末高熵合金，研究了球磨预处理工艺对粉末高熵合金显微组织和拉伸性能的影响。结果表明，预合金粉末的球形度随球磨时间的延长不断降低；烧结态高熵合金的物相组成不随球磨参数改变，始终为单一面心立方结构；球磨时间的延长和球料比的增加都会降低高熵合金的晶粒尺寸。随着球磨能量的升高，合金屈服强度不断增大，球料比为7.5:1.0、球磨时长为100 h时，合金屈服强度达到最高，提升约19%，强化贡献主要源于细晶强化；合金抗拉强度先增大后减小，球料比为7.5:1.0、球磨时长为30 h时，合金抗拉强度提升最大，提升约为12%。
Abstract:CoCrFeMnNi high-entropy alloys with nearly full density were fabricated by spark plasma sintering (SPS) process. The effects of mechanical milling on the microstructure and tensile properties of the CoCrFeMnNi alloys were investigated. The results show that the sphericity of the pre-alloyed powders decreases with the milling time increasing. The phase composition of as-SPSed alloys presents a single face-centered cubic structure, and the grain size decreases with the increase of ball-to-powder weight ratio and mechanical milling time. Compared with the alloys without mechanical milling, the yield strength of the as-SPSed alloys increases with the increase of mechanical milling energy, which reaches the highest value when the ball-to-powder weight ratio is 7.5:1.0 and the mechanical milling time is 100 h, increasing by about 19%, which is mainly due to the fine grain strengthening. The ultimate tensile strength tends to firstly increase and then decrease, which reaches the highest value when the ball-to-powder weight ratio is 7.5:1.0 and the mechanical milling time is 30 h, increasing by about 12%.
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图 1 CoCrFeMnNi高熵合金粉末原始显微形貌
Figure 1. Microstructure of the original CoCrFeMnNi high-entropy alloy powders
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图 3 球磨过程粉末形貌显微：（a）～（c）球料比5.0:1.0，球磨30、50和100 h；（d）～（f）球料比7.5:1.0，球磨30、50和100 h
Figure 3. SEM images of the presenting powders during mechanical milling: (a)~(c) R=5.0:1.0, milling for 30, 50, and 100 h; (d)~(f) R=7.5:1.0, milling for 30, 50, and 100 h
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图 4 不同球磨参数烧结样品X射线衍射图谱
Figure 4. XRD patterns of the as-SPSed CoCrFeMnNi alloys with different mechanical milling parameters
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图 5 不同球磨参数对应烧结态合金显微组织及晶粒尺寸：（a）未球磨；（b）30 h，球料比5.0:1.0；（c）30 h，球料比7.5:1.0；（d）100 h，球料比5.0:1.0；（e）100 h，球料比7.5:1.0；（f）晶粒尺寸分布
Figure 5. Microstructures and grain size of the as-SPSed alloys in the different mechanical milling parameters: (a) without mechanical milling; (b) 30 h, R=5.0:1.0; (c) 30 h, R=7.5:1.0; (d) 100 h, R=5.0:1.0; (e) 100 h, R=7.5:1.0; (f) distribution of the average grain size
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图 6 不同球磨参数下烧结态合金拉伸性能
Figure 6. Tensile properties of the as-SPSed alloys corresponding to different mechanical milling parameters
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图 7 不同球磨参数下强化机制的贡献
Figure 7. Contribution of strengthening mechanisms under the different mechanical milling parameters
表 1 初始CoCrFeMnNi粉末化学成分（原子分数）
Table 1 Chemical compositions of the original CoCrFeMnNi powders
% Co Cr Fe Mn Ni 20.35 18.49 20.04 20.83 20.24 
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表 2 烧结态合金力学性能
Table 2 Tensile properties of the as-SPSed alloys
球磨时长 / h 球料比 屈服强度 /
MPa抗拉强度 /
MPa延伸率 / % 0 — 280 550 51 30 5.0:1.0 283 563 51 30 7.5:1.0 295 615 56 100 5.0:1.0 301 551 58 100 7.5:1.0 342 527 54
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