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磁性高熵合金在能量转换、磁滞电机、电磁控制机构等相关领域具有一定的应用前景. 采用选区激光熔化(SLM)成形技术在不同工艺参数下制备出AlCoCrCuFeNi高熵合金, 对合金的相组成、微观组织结构、磁性能和微观力学行为进行了系统的研究. 结果表明, SLM成形态合金主要由体心立方(BCC)基体相和少量近似球形的面心立方(FCC)纳米析出相组成, 其纳米硬度随着激光功率的增加而减小, 随着扫描速度的变化在一定范围波动, 但是整体均呈现出优异的微观力学性能, 且其纳米压痕蠕变变形机制异于传统经典蠕变理论, 主要受位错运动控制. SLM成形态合金均表现出典型的半硬磁特性, 其饱和磁化强度受SLM工艺参数影响较小, 保持在43 A·m2/kg左右; 矫顽力随着激光功率的增加从1.72 kA/m增加到2.71 kA/m, 随着扫描速度的增加从2.37 kA/m减小到1.98 kA/m. 磁性能研究表明, 该成形态AlCoCrCuFeNi高熵合金的磁性能有望广泛应用于磁控机构等领域. 本工作可为后续优化SLM高熵合金的综合磁学性能以及纳米压痕室温蠕变机制提供一定的理论基础和实实验方向.
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关键词:
- 选区激光熔化 /
- AlCoCrCuFeNi高熵合金 /
- 半硬磁特性 /
- 微观力学
Magnetic high-entropy alloy (HEA) has certain application prospects in the fields of energy conversion, hysteresis motor, electromagnetic control mechanism and others. In this study, AlCoCrCuFeNi HEA is prepared by selective laser melting (SLM) with different process parameters, and the phase composition, microstructure, magnetic properties and micromechanical behavior are studied systematically. The results show that the SLMed alloy mainly consists of a BCC matrix phase with a small quantity of approximately spherical FCC precipitated nanophase. The nanohardness decreases with the increase of laser power and fluctuates in a certain range with the change of scanning speed, but the whole sample shows excellent micromechanical properties. Besides, it is found that the room-temperature nanoindentation creep deformation mechanism of AlCoCrCuFeNi HEAs is mainly controlled by dislocation motion, which is different from the results given by the traditional classical creep theory. Both of SLMed alloys exhibit typical semi-hard magnetic properties. The saturation magnetization is affected slightly by the SLM process parameters and remains at about 43 A·m2/kg because all samples have a similar quantity of ferromagnetic elements (Fe,Co and Ni). However, the coercivity increases from 1.72 to 2.71 kA/m with the increase of laser power (P), and decreases from 2.37 to 1.98 kA/m with the increase of scanning speed (v), which can be attributed to the different effects of porosity and internal stress on the pinning of domain walls under different process parameters (P and v). This work provides a theoretical basis and experimental direction for further studying the optimization of comprehensive magnetic properties and the room temperature creep mechanism of SLMed high-entropy alloy.-
Keywords:
- selective laser melting /
- AlCoCrCuFeNi high-entropy alloy /
- semi-hard magnetic property /
- micro-mechanical behavior
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图 1 SLM成形设备(a)、SLM工艺示意图(b)及SLM成形样品顶面实物图(c)
Fig. 1. SLM equipment (a), schematic diagram of the SLM process (b) and the top-view physical picture of SLMed alloys.
图 2 SLM成形态AlCoCrCuFeNi高熵合金在不同工艺参数下的孔隙率变化
Fig. 2. Variation of porosity with laser power and scanning speed of the SLMed AlCoCrCuFeNi HEAs.
图 3 不同工艺参数下制备的SLM成形态AlCoCrCuFeNi高熵合金的XRD图谱 (a) 激光扫描速率为1450 mm/s, 激光功率为110—150 W; (b) 激光功率为130 W, 激光扫描速率为1350—1550 mm/s
Fig. 3. The XRD spectra of SLMed samples, (a) processed at 1450 mm/s laser scanning and different laser power (110–150 W), (b) processed at 130 W laser power and different (1350–1550 mm/s) laser scanning speed, respectively.
图 4 SLM成形态试样的典型微观结构 (a), (b) SEM形貌图; (c), (d) TEM明场像图; (e), (f) 选区电子衍射图; (g)表示位错堆积和缠结的TEM明场像图
Fig. 4. Typical microstructures of SLMed samples: (a), (b) SEM images; (c), (d) bright-field TEM images; (e), (f) the selective area electron diffraction; (g) TEM bright field image showing the dislocation pile up and entanglement.
图 5 SLM成形态AlCoCrCuFeNi高熵合金在不同激光功率下的磁滞回线(a)(插图为局部放大图)和磁性参数(b)的变化规律
Fig. 5. Hysteresis loops (a) and variation in Ms, Hc (b) of SLMed AlCoCrCuFeNi specimens at different power, respectively. The illustration is partial enlargement of panel (a)
图 6 SLM成形态AlCoCrCuFeNi高熵合金在不同扫描速率下的磁滞回线(a) (插图为局部放大图)和磁性参数(b)的变化规律
Fig. 6. Hysteresis loops (a) and the variation in Ms, Hc (b) of SLMed AlCoCrCuFeNi specimens at different scanning speed, respectively; the illustration is partial enlargement of Figure (a)
图 7 纳米压痕实验. 不同激光扫描速度(a)和激光功率(b)条件下打印态试样的压痕深度-载荷关系曲线
Fig. 7. Nanoindentation test. The curves of load on surface vs. displacement into surface of printed samples with different P (a) and v (b).
图 8 纳米压痕实验 (a)压痕深度和载荷关系曲线; (b)拟合蠕变曲线
Fig. 8. Nanoindentation test: (a) Curve of load on surface vs. displacement into surface; (b) fitting creep curve.
表 1 AlCoCrCuFeNi粉末的化学成分及各元素的特征参数
Table 1. Chemical compositions and element-characteristic parameters of the AlCoCrCuFeNi powders.
Elements Al Co Cr Cu Fe Ni Mass fraction/% 8.85 18.86 16.59 20.28 17.25 18.11 density/(g·mm–3) 2.7 8.85 7.75 8.90 7.87 8.85 Melting point/K 933 1770 2123 1356 1811 1728 Average atomic/nm 0.1432 0.1363 0.1249 0.1280 0.1270 0.1240 Structure FCC HCP BCC FCC BCC FCC VEC* 3 9 6 11 8 10 *VEC—valence electron concentration. 
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表 2 SLM制备AlCoCrCuFeNi高熵合金的工艺参数
Table 2. Process parameters of fabricating AlCoCrCuFeNi HEAs using SLM technique.
工艺参数 取值 Laser thickness (t)/μm 40 Laser power (P)/W 110—150 Scan velocity (v)/(mm·s–1) 1350—1550 Hatch spacing (h)/μm 50
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表 3 不同激光功率(P)下SLM成形态AlCoCrCuFeNi高熵合金的XRD参数
Table 3. The XRD parameters of SLMed AlCoCrCuFeNi HEAs at different laser power.
P/W VBCC/% VFCC/% aBCC/Å aFCC/Å 110 94.89 5.11 2.8709±0.0006 3.6100±0.0006 120 94.38 5.62 2.8726±0.0017 3.6280±0.0007 130 94.24 5.76 2.8752±0.0012 3.6289±0.0017 140 93.41 6.59 2.8762±0.0011 3.6310±0.0023 150 92.04 7.96 2.8763±0.0006 3.6367±0.0014
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表 4 不同扫速(v)下SLM成形态AlCoCrCuFeNi高熵合金的XRD参数
Table 4. The XRD parameters of SLMed AlCoCrCuFeNi HEAs at different laser scanning.
v/(mm·s–1) VBCC/% VFCC/% aBCC/(Å aFCC/Å 1350 94.84 5.16 2.8840±0.0029 3.6460±0.0012 1400 94.89 5.11 2.8825±0.0012 3.6289±0.0017 1450 93.75 6.25 2.8810±0.0034 3.6430±0.0006 1500 94.13 5.87 2.8773±0.0015 3.6358±0.0021 1550 93.62 6.38 2.8737±0.0009 3.6297±0.0024
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表 5 不同激光功率下合金的纳米压痕参数
Table 5. Nanoindentation of alloys at different laser power.
P/W Hmax /nm Nano-hardness/GPa E/GPa 110 321.5±13.8 8.8±0.9 202.3±8.4 120 322.4±2.1 8.7±0.2 202.5±6.7 130 323.2±13.6 8.7±0.8 208.9±15.6 140 326.8±6.2 8.5±0.5 201.8±2.3 150 332.3±8.4 8.2±0.5 203.8±5.0
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表 6 不同激光扫描速度下合金的纳米压痕参数
Table 6. Nanoindentation of alloys at different laser scanning speed.
v/(mm·s–1) Hmax /nm Nano-hardness/GPa E/GPa 1350 331.0±6.3 8.2±0.4 199.2±10.9 1400 323.2±13.6 8.7±0.8 208.9±15.6 1450 322.3±3.8 8.8±0.2 201.7±8.6 1500 338.7±8.5 7.7±0.4 197.0±7.7 1550 332.3±8.4 8.1±0.5 193.3±5.0
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