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The influence of ball milling processing variables on the microstructure and compaction behavior of Fe–Mn–Cu alloys


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Fig. 1

SEIs of the as-received (A) Fe, (B) Mn, and (C) Cu powders used in the present study. SEI, secondary electron image
SEIs of the as-received (A) Fe, (B) Mn, and (C) Cu powders used in the present study. SEI, secondary electron image

Fig. 2

SEIs of the size and shape of the selected processed alloy powders: (A) BD5-1; (B) BD5-3; and (C) BD5-4 alloys. SEI, secondary electron image
SEIs of the size and shape of the selected processed alloy powders: (A) BD5-1; (B) BD5-3; and (C) BD5-4 alloys. SEI, secondary electron image

Fig. 3

Results of EDS analysis of the alloys in powder form: (A–C) BD5-1; (D–F) BD5-3; (G–I) BD5-4. EDS, energy dispersive spectroscopy
Results of EDS analysis of the alloys in powder form: (A–C) BD5-1; (D–F) BD5-3; (G–I) BD5-4. EDS, energy dispersive spectroscopy

Fig. 4

The distribution of particle size for BD5-1, BD5-2, BD5-4, BD5-9, BD5-10, and BD5-11 alloys. d, diameter
The distribution of particle size for BD5-1, BD5-2, BD5-4, BD5-9, BD5-10, and BD5-11 alloys. d, diameter

Fig. 5

XRD patterns of all powder samples: (A) BD0-1 to BD0-6; (B) BD5-7 to BD5-12; (C) BD5-13 to BD5-19; (D) BD10-20 to BD10-25. CPS, counts/s; XRD, X-ray diffraction
XRD patterns of all powder samples: (A) BD0-1 to BD0-6; (B) BD5-7 to BD5-12; (C) BD5-13 to BD5-19; (D) BD10-20 to BD10-25. CPS, counts/s; XRD, X-ray diffraction

Fig. 6

The experimental results of RD versus CP for [(Fe–35 wt%Mn)95–Cu5] green samples. CP, compaction pressure; RD, relative density
The experimental results of RD versus CP for [(Fe–35 wt%Mn)95–Cu5] green samples. CP, compaction pressure; RD, relative density

Fig. 7

EDS analysis results of the compacted samples: (A–C) BD5-1; (D–F) BD5-3; and (G–I) BD5-4. EDS, energy dispersive spectroscopy
EDS analysis results of the compacted samples: (A–C) BD5-1; (D–F) BD5-3; and (G–I) BD5-4. EDS, energy dispersive spectroscopy

Fig. 8

EDS analysis results of the green samples: (A–C) BD5-9; (D–F) BD5-10; and (G–I) BD5-11. EDS, energy dispersive spectroscopy
EDS analysis results of the green samples: (A–C) BD5-9; (D–F) BD5-10; and (G–I) BD5-11. EDS, energy dispersive spectroscopy

Fig. 9

ANOVA results of RD: (A) The experimental and the predicted values of RD; and (B) normal probability of residuals of RD of the developed compacted samples. RD, relative density
ANOVA results of RD: (A) The experimental and the predicted values of RD; and (B) normal probability of residuals of RD of the developed compacted samples. RD, relative density

Fig. 10

The impact of the input variables on the RD of the developed green samples: (A, C, E, G, I, K) 3D surface plots; (B, D, F, H, J, L) 2D contour plots. RD, relative density
The impact of the input variables on the RD of the developed green samples: (A, C, E, G, I, K) 3D surface plots; (B, D, F, H, J, L) 2D contour plots. RD, relative density

The results of the ANOVA test performed for the lattice strain

Source Sum of squares DF Mean square F-value p-value
Model 0.1630 10 0.0163 2.49 0.0499
MT 0.0855 1 0.0855 13.08 0.0023
BPMR 0.0128 1 0.0128 1.96 0.1807
MS 0.0147 1 0.0147 2.25 0.1532
CC 0.0092 1 0.0092 1.41 0.2518
(MT) × (BPMR) 0.0074 1 0.0074 1.13 0.3032
(MT) × (MS) 0.0298 1 0.0298 4.55 0.0487
(MT) × (CC) 0.0013 1 0.0013 0.1983 0.6621
(BPMR) × (MS) 0.0019 1 0.0019 0.2962 0.5938
(BPMR) × (CC) 0.0003 1 0.0003 0.0442 0.8361
(MS) × (CC) 0.0001 1 0.0001 0.0169 0.8983
Residual 0.1046 16 0.0065
Lack of fit 0.1045 14 0.0075 355.54 0.0028
Pure error 0.0000 2 0.0000
Total 0.2676 26

The results of ANOVA test performed for the RD

Source Sum of squares DF Mean square F-value p-value
Model 274.0800 10 27.4100 12.2300 <0.0001
MT 50.7600 1 50.7600 22.6400 0.0002
BPMR 37.1000 1 37.1000 16.5500 0.0009
MS 102.2000 1 102.2000 45.5900 <0.0001
CC 50.0200 1 50.0200 22.3100 0.0002
(MT) × (BPMR) 6.4300 1 6.4300 2.8700 0.1098
(MT) × (MS) 0.5041 1 0.5041 0.2249 0.6418
(MT) × (CC) 19.7600 1 19.7600 8.8100 0.0090
(BPMR) × (MS) 3.1000 1 3.1000 1.3800 0.2570
(BPMR) × (CC) 3.4800 1 3.4800 1.5500 0.2308
(MS) × (CC) 0.7396 1 0.7396 0.3299 0.5737
Residual 35.8700 16 2.2400
Lack of fit 35.6100 14 2.5400 20.1700 0.0482
Pure error 0.2522 2 0.1261
Total 309.9500 26

Design input parameters (MT, MS, BPMR, and CC) and experimental results (RD, crystallite size, and lattice strain) obtained in the present study

Exp. no. Alloy code MT, h BPMR, n MS, rev/min CC, wt% RD, % Crystallite size (from Fe peak), nm Lattice strain (from Fe peak), %
1 BD0-1 5.5 10 100 0 71.65 37.0 0.3120
2 BD0-2 5.5 10 300 0 65.94 28.0 0.3340
3 BD0-3 1.0 10 200 0 66.63 32.0 0.3030
4 BD0-4 10.0 10 200 0 67.76 25.0 0.3730
5 BD0-5 5.5 5 200 0 67.99 44.0 0.2850
6 BD0-6 5.5 15 200 0 68.53 25.0 0.3760
7 BD5-1 1.0 5 200 5 75.04 58.0 0.1650
8 BD5-2 10.0 5 200 5 72.66 18.0 0.5070
9 BD5-3 1.0 15 200 5 73.49 38.0 0.2480
10 BD5-4 10.0 15 200 5 66.04 22.0 0.4180
11 BD5-5 5.5 5 100 5 75.46 58.0 0.1650
12 BD5-6 5.5 15 100 5 72.08 28.0 0.3340
13 BD5-7 5.5 5 300 5 71.20 41.0 0.2740
14 BD5-8 5.5 15 300 5 64.30 26.0 0.3550
15 BD5-9 1.0 10 100 5 75.19 58.0 0.1670
16 BD5-10 10.0 10 100 5 71.79 17.0 0.5560
17 BD5-11 1.0 10 300 5 70.98 21.0 0.4610
18 BD5-12 10.0 10 300 5 66.16 18.0 0.5050
19 BD5-13 5.5 10 200 5 69.66 22.0 0.4180
20 BD10-1 5.5 10 100 10 75.23 25.0 0.3740
21 BD10-2 5.5 10 300 10 67.80 23.0 0.4080
22 BD10-3 1.0 10 200 10 75.08 33.0 0.3360
23 BD10-4 10.0 10 200 10 67.32 28.0 0.3340
24 BD10-5 5.5 5 200 10 75.38 23.0 0.4080
25 BD10-6 5.5 15 200 10 72.19 24.0 0.4580
26 BD5-13R 5.5 10 200 5 68.99 22.0 0.4180
27 BD5-13R 5.5 10 200 5 69.12 22.0 0.4180

The results of particle size analysis for selected alloys

Alloy code Average particle size, nm Standard deviation, nm % intensity (main peak) PDI
BD5-1 1,477.00 480.50 96.50 0.33
BD5-2 655.40 220.30 91.20 0.49
BD5-4 327.10 53.28 100.00 0.52
BD5-9 1,274.00 315.90 96.20 0.42
BD5-10 638.70 214.10 91.10 0.41
BD5-11 499.50 129.40 99.10 0.35

The results of the ANOVA test performed for the crystallite size

Source Sum of squares DF Mean square F-value p-value
Model 2.696 × 105 10 26,963.56 3.89 0.0079
MT 1.025 × 105 1 1.025 × 105 14.78 0.0014
BPMR 56,033.33 1 56,033.33 8.08 0.0118
MS 33,920.33 1 33,920.33 4.89 0.0419
CC 12,610.08 1 12,610.08 1.82 0.1963
(MT) × (BPMR) 14,520.25 1 14,520.25 2.09 0.1672
(MT) × (MS) 36,100.00 1 36,100.00 5.20 0.0366
(MT) × (CC) 144.00 1 144.00 0.0208 0.8872
(BPMR) × (MS) 5,402.25 1 5,402.25 0.7789 0.3906
(BPMR) × (CC) 7,225.00 1 7,225.00 1.04 0.3226
(MS) × (CC) 1,190.25 1 1,190.25 0.1716 0.6842
Residual 1.110E × 105 16 6,936.07
Lack of Fit 1.109E × 105 14 7,923.37 316.93 0.0031
Pure Error 50.00 2 25.00
Total 3.806 × 105 26
eISSN:
2083-134X
Język:
Angielski
Częstotliwość wydawania:
4 razy w roku
Dziedziny czasopisma:
Materials Sciences, other, Nanomaterials, Functional and Smart Materials, Materials Characterization and Properties