Preparasi Serbuk dan Sintering Magnet Permanen Barium Heksaferit dengan Aditif FeMn

56

LAMPIRAN 1
ALAT DAN BAHAN PENELITIAN

1. Peralatan Penelitian

Mortar dan Alu

High Energy milling (HEM)

Jar mill (untuk HEM)

Ayakan 100 mesh

Saringan

Ball mill (untuk HEM)

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57

Particle Size Analyzer (PSA)

SEM-EDX

Vacuum Furnace

Magnetizer K-Series

X-Ray Diffraction

Spatula
Neraca Digital

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58

Peralatan Archimedes


Molding

Beaker Glass

Dryer

piknometer

Kertas Label

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59

Bata tahan panas

Microhardness tester

Hydraulic press


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60

2. Bahan Penelitian

Serbuk BaFe12O19

Seluna

Serbuk FeMn

Toluen

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61

LAMPIRAN 2

DATA-DATA HASIL PENGUKURAN DENSITAS

1. True Density
Mengukur true density dengan menggunakan rumus :

ρs

= true density sampel (g/cm3)

m1

= massa piknometer kosong (g)

m2

= massa piknometer diisi media cair (g)

m3

= massa piknometer diisi serbuk (g)


m4

= massa piknometer diisi sampel serbuk dan media cair (g)

ρmedia cair = densitas media cair (g/cm3)
1.1 True density eksperimen
1. True density BaFe12O19 + FeMn milling 15 menit.
Komposisi
Fe-Mn
(wt%)

m (g)

m (g)

m (g)

m (g)


m m (g)

m m (g)

m m (g)

ρ
ρ
toluen sampel
(g/cm³) (g/cm³)

0,5
1
3
5
10

9,813
9,813
9,813

9,813
9,813

18,550
18,550
18,550
18,550
18,550

10,802
10,803
10,806
10,803
10,792

19,372
19,366
19,373
19,368
19,352


0,989
0,990
0,993
0,990
0,979

8,737
8,737
8,737
8,737
8,737

8,570
8,563
8,567
8,565
8,560

0,8669

0,8669
0,8669
0,8669
0,8669

5,134
4,932
5,064
4,990
4,795

2. True density BaFe12O19 + FeMn milling 30 menit.
Komposisi
Fe-Mn
(wt%)

m (g)

m (g)


m (g)

m (g)

m m (g)

m m (g)

m m (g)

ρ
ρ
toluen sampel
(g/cm³) (g/cm³)

0,5
1
3
5
10


9,813
9,813
9,813
9,813
9,813

18,550
18,550
18,550
18,550
18,550

10,801
10,807
10,807
10,806
10,802

19,369
19,38
19,378
19,372
19,364

0,988
0,994
0,994
0,993
0,989

8,737
8,737
8,737
8,737
8,737

8,568
8,573
8,571
8,566
8,562

0,8669
0,8669
0,8669
0,8669
0,8669

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5,068
5,254
5,191
5,034
4,899

62

3. True density serbuk awal BaFe12O19 dan FeMn
ρs
(g/cm3)
5,2
7,7

Sampel
BaFe12O19
FeMn

1.2 True density teori
Pengukuran true density teori dilakukan dengan menggunakan rumus sebagai berikut
:
(

Keterangan :
ρx , ρy

)

= Densitas sampel (g/cm3)

%wtx , %wty = komposisi sampel (wt%)

wt %
BaFe O ₉
99,5
99
97
95
90

wt %
Fe-Mn
0,5
1
3
5
10

ρ
BaFe O ₉
(g/cm³)
5,2
5,2
5,2
5,2
5,2

ρ FeMn
(g/cm³)

ρ Teori
Sampel
(g/cm³)

7,7
7,7
7,7
7,7
7,7

5,208
5,217
5,251
5,286
5,374

2. Bulk Density
Mengukur bulk density dari sampel berbentuk pelet menggunakan rumus :

Keterangan :
ρs

= bulk density sampel (g/cm3)

mk

= massa kering sampel (g)

mb

= massa basah sampel (g)

ρmedia cair = densitas media cair (g/cm3)

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Waktu
Milling

15
menit

30
menit

Komposisi
FeMn
(wt%)
0,5
1
3
5
10
0,5
1
3
5
10

mk (g)
0,341
0,168
0,284
0,157
0,298
0,159
0,217
0,43
0,183
0,157

mb (g)

mkmb (g)

0,27
0,131
0,22
0,12
0,222
0,125
0,17
0,335
0,14
0,119

0,071
0,037
0,064
0,037
0,076
0,034
0,047
0,095
0,043
0,038

ρ air
(g/cm3)
0,9962
0,9962
0,9962
0,9962
0,9962
0,9962
0,9962
0,9962
0,9962
0,9962

ρ sampel
(g/cm3)
4,784566
4,523286
4,420638
4,227119
3,906153
4,6587
4,599477
4,509116
4,239642
4,115879

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64

LAMPIRAN 3
DATA PENGUKURAN DIAMETER PARTIKEL SERBUK DENGAN
MENGGUNAKAN SOFTWARE IMAGE-J

1. BaFe12O19 milling 30 menit
Area
(µm)
1.284
1.47
1.565
2.39
2.511
2.803
3.733
8.632
11.179
12.571
23.075
26.391

Min

Max

% Area

255
255
255
255
255
255
255
255
255
255
255
255
255
255
255
255
255
255
255
255
255
255
255
255
Diameter rata - rata

100
100
100
100
100
100
100
100
100
100
100
100

Diameter
(µm)
1.133137
1.212436
1.251
1.545962
1.584614
1.674216
1.932097
2.938027
3.343501
3.545561
4.803644
5.137217
2.508451

2. BaFe12O19 + FeMn 5 % milling 30 menit
Area
Min
Max
(µm)
1.289
255
255
1.51
255
255
1.721
255
255
2.184
255
255
3.019
255
255
7.145
255
255
8.261
255
255
8.99
255
255
9.531
255
255
10.203
255
255
12.838
255
255
15.135
255
255
21.743
255
255
Diameter rata – rata

% Area
100
100
100
100
100
100
100
100
100
100
100
100
100

Diameter
(µm)
1.135341
1.228821
1.311869
1.477836
1.737527
2.673013
2.874196
2.998333
3.087232
3.194214
3.583015
3.890373
4.662939
2.604208

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65

LAMPIRAN 4
DATA HASIL ANALISIS XRD

1. Serbuk BaFe12O19

Raw Data
General information

Analysis date

2017/03/16 13:54:07

Sample name

BaO6Fe2O3

Measurement date

2017/03/14 09:31:44

File name

BaO6Fe2O3.ras

Operator

administrator

Comment

Measurement conditions

X-Ray

40 kV , 30 mA

Scan speed / Duration time

2.0000 deg/min

Goniometer
Attachment
Filter
CBO selection slit
Diffrected beam mono.
Detector
Scan mode

SmartLab(In-plane)
RxRy
Cu_K-beta
BB
None
SC-70
CONTINUOUS

Step width
Scan axis
Scan range
Incident slit
Length limiting slit
Receiving slit #1
Receiving slit #2

0.0100 deg
Theta/2-Theta
10.0000 - 90.0000 deg
2/3deg
10.0mm
2/3deg
0.450mm

Measurement profile

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Meas. data:BaO6Fe2O3
Calc. data:BaO6Fe2O3

200

Intensity (counts)

150

100

50

0

20

40

60

80

2-theta (deg)

2. Serbuk BaFe12O19 + FeMn 1% milling 15 menit

Raw Data
General information

Analysis date

2017/03/16 14:11:33

Sample name

BaO6Fe2O3 99%+FeMn 1%

Measurement date

2017/03/14 10:13:53

File name

BaO6Fe2O3 99%+FeMn 1%.ras

Operator

administrator

Comment

Measurement conditions
X-Ray

40 kV , 30 mA

Scan speed / Duration time

2.0000 deg/min

Goniometer
Attachment
Filter
CBO selection slit
Diffrected beam mono.
Detector
Scan mode

SmartLab(In-plane)
RxRy
Cu_K-beta
BB
None
SC-70
CONTINUOUS

Step width
Scan axis
Scan range
Incident slit
Length limiting slit
Receiving slit #1
Receiving slit #2

0.0100 deg
Theta/2-Theta
10.0000 - 90.0000 deg
2/3deg
10.0mm
2/3deg
0.450mm

Measurement profile

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Meas. data:BaO6Fe2O3 99%+FeMn 1%
Calc. data:BaO6Fe2O3 99%+FeMn 1%

200

Intensity (counts)

150

100

50

0

20

40

60

80

2-theta (deg)

3. Serbuk BaFe12O19 + FeMn 5 % milling 15 menit

Raw Data
General information

Analysis date

2017/03/16 14:04:01

Sample name

BaO6Fe2O3 95%+FeMn 5%

Measurement date

2017/03/14 10:55:52

File name

BaO6Fe2O3 95%+FeMn 5%.ras

Operator

administrator

Comment

Measurement conditions
40 kV , 30 mA

Scan speed / Duration time

2.0000 deg/min

SmartLab(In-plane)
RxRy
Cu_K-beta
BB
None
SC-70
CONTINUOUS

Step width
Scan axis
Scan range
Incident slit
Length limiting slit
Receiving slit #1
Receiving slit #2

0.0100 deg
Theta/2-Theta
10.0000 - 90.0000 deg
2/3deg
10.0mm
2/3deg
0.450mm

X-Ray
Goniometer
Attachment
Filter
CBO selection slit
Diffrected beam mono.
Detector
Scan mode

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Measurement profile
Meas. data:BaO6Fe2O3 95%+FeMn 5%
Calc. data:BaO6Fe2O3 95%+FeMn 5%

Intensity (counts)

150

100

50

0

20

40

60

80

2-theta (deg)

4. BaFe12O19 + FeMn 10% milling 15 menit

Raw Data
General information
Analysis date

2017/03/16 14:00:23

Sample name

BaO6Fe2O3 90%+FeMn 10%

Measurement date

2017/03/14 11:37:52

File name

BaO6Fe2O3 90%+FeMn 10%.ras

Operator

administrator

Comment

Measurement conditions
X-Ray

40 kV , 30 mA

Scan speed / Duration time

2.0000 deg/min

Goniometer
Attachment
Filter
CBO selection slit
Diffrected beam mono.
Detector
Scan mode

SmartLab(In-plane)
RxRy
Cu_K-beta
BB
None
SC-70
CONTINUOUS

Step width
Scan axis
Scan range
Incident slit
Length limiting slit
Receiving slit #1
Receiving slit #2

0.0100 deg
Theta/2-Theta
10.0000 - 90.0000 deg
2/3deg
10.0mm
2/3deg
0.450mm

Measurement profile

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69

Meas. data:BaO6Fe2O3 90%+FeMn 10%
Calc. data:BaO6Fe2O3 90%+FeMn 10%

150

Intensity (counts)

100

50

0

20

40

60

80

2-theta (deg)

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70

LAMPIRAN 5
DATA HASIL PENGUJIAN HARDNESS VICKERS

1. BaFe12O19 99,5 wt% + FeMn 0,5 wt% milling 15 menit.

2. BaFe12O19 99 wt% + FeMn 1 wt% milling 15 menit.

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71

3. BaFe12O19 99,5 wt% + FeMn 3 wt% milling 15 menit.

4. Serbuk BaFe12O19 + FeMn 5 wt% milling 15 menit.

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72

5. Serbuk BaFe12O19 + FeMn 10 wt% milling 15 menit.

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6. BaFe12O19 99,5 wt% + FeMn 0,5 wt% milling 30 menit.

7. BaFe12O19 99 wt% + FeMn 1 wt% milling 30 menit.

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8. BaFe12O19 97 wt% + FeMn 3 wt% milling 30 menit.

9. BaFe12O19 95 wt% + FeMn 5 wt% milling 30 menit.

10. BaFe12O19 90 wt% + FeMn 10 wt% milling 30 menit.

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75

LAMPIRAN 6
DATA HASIL ANALISIS VSM

1. Sampel pelet BaFe12O19 milling 15 menit.

2. Sampel pelet BaFe12O19 milling 30 menit.

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76

3. Sampel pelet BaFe12O19 + FeMn 5 wt%milling 30 menit.

4. Sampel pelet BaFe12O19 + FeMn 5 wt%milling 15 menit.

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77

5. Sampel serbuk BaFe12O19 + 5 wt % FeMn milling 15 menit

6. Sampel serbuk BaFe12O19 + 1 wt % FeMn milling 15 menit

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78

7. Sampel serbuk BaFe12O19 +10 wt % FeMn milling 15 menit

8. Sampel serbuk BaFe12O19 + 1 wt % FeMn milling 30 menit

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79

9. Sampel serbuk BaFe12O19 + 5 wt % FeMn milling 30 menit

10. Sampel serbuk BaFe12O19 + 10 wt % FeMn milling 30 menit

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80

LAMPIRAN 7
DATA HASIL PENGUKURAN BH MAX

1. Sampel Serbuk
a. BaFe12O19+ FeMn 1 wt% milling 15 menit.

15 min FeMn 1 %

600000

400000

200000

0
0

15 min
FeMn 1
%
y = 1E-07x4 - 0.0005x3 0.1123x2 + 1008.1x +
4225.9
500 1000 1500R²2000
=1

569600
569580
569560
569540
569520
569500
569480
569460
569440
569420
569400
569380
569360
569340
569320
569300
569280
569260
569240
569220
569200
569180
569160
569140
569120
569100
569080
569060
569040
569020
569000

BH
Poly. (BH)
Linear (BH)
y = 1E-07x4 - 0.0005x3 - 0.1123x2 +
1008.1x + 4225.9
800

900

1000

1100

b. BaFe12O19+ FeMn 5 wt% milling 15 menit.

15 min FeMn 5 %

250000
200000

15 min
FeMn 5 %

150000
100000
50000
0
0

500

Poly. (15
min FeMn
y = -0.108x2 + 298.97x +
5 %)
6075.9
=1
1000 1500 R²
2000

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81

BH 5 % FeMn 15 min
214000
213000
212000
211000
210000
209000
208000
207000
206000
205000
204000
203000
202000
201000
200000

BH 5 %
FEMN
Poly. (BH 5 %
FEMN)

0

500

y = -0.108x2 + 298.97x + 6075.9
1000
1500 R² =2000
1

c. BaFe12O19 + FeMn 10 wt% milling 15 menit.

15 min FeMn 10 %

600000
500000
400000
300000
200000
100000
0
0

200

400

600

15 min
FeMn 10 %
800

BH 15 Min 10 % FeMn
555000
554000
553000
552000
551000
550000
549000
548000
547000
546000
545000
544000
543000
542000
541000
540000

BH 15 Min 10 %
FeMn
Poly. (BH 15 Min
10 % FeMn)

0

200

y = -0.0332x3 + 42.763x2 - 16175x + 2E+06
400
600 R² = 1 800

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d. BaFe12O19 + FeMn 1 wt% milling 30 menit.

500000

30 min 1 % FeMn

400000
30 min 1
% FeMn

300000
200000

Poly. (30
min 1 %
FeMn)

100000
0
0

500

1000

1500

BH 30 min 1 % FeMn

426000
425000
424000
423000
422000
421000
420000
419000
418000
417000
416000
415000
414000
413000
412000
411000
410000
409000
408000

BH
Poly. (BH)

0

500

y = -0.6759x2 + 1071.4x - 3948
1000
R² = 0.9997 1500

e. BaFe12O19 + FeMn 5 wt% milling 30 menit.

30 min 5 % FeMn

600000
400000
200000
0
0

500

1000

30 min 5 %
FeMn
1500

BH 5 % FeMn 30 min

486000
485800
485600
485400
485200
485000
484800
484600
484400
484200
484000
483800
483600
483400
483200
483000
482800
482600
482400
482200
482000

BH 5 % FeMn
30 min
y = 9E-08x4 - 0.0003x3 - 0.3893x2 +
1052.7x + 5.8988
Poly. (BH 5 %
R² = 1
FeMn 30 min)
0

500

1000

1500

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f. BaFe12O19 + FeMn 10 wt% milling 30 menit.

30 min 10 % FeMn
400000
300000
200000
100000

30 min 10 %
FeMn

0
0

500

1000

1500

-0.4385x
+ 719.89x + 24325
BH 30 miny =10%
FeMn
2

R² = 1

322000
320000
318000
316000
314000
312000
310000
308000
306000
304000
302000
300000
298000
296000
294000
292000
290000

BH 30 min 5%
FeMn
Poly. (BH 30
min 5%
FeMn)
0

500

1000

1500

2. Sampel Pelet
a. BaFe12O19 milling 15 menit.

B vs H

500000
400000
300000

BH

200000

Poly. (BH)
100000
0
0

200

400

y = -2.9658x2 + 4149.9x - 1E+06
R² = 1
600
800
1000

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397000
396000
395000
394000
393000
392000
391000
390000
389000
388000
387000
386000
385000
384000
383000
382000
381000
380000

BH max

BH
Poly. (BH)

0

y = -2.9658x2 + 4149.9x - 1E+06
400
600 R² 800
1000
=1

200

b. BaFe12O19 milling 30 menit.

BH max

400000
300000
200000

BH max
Poly. (BH max)
y = -1.9714x2 + 3124.5x - 887889
R² = 1

100000
0
0

200

350600
350500
350400
350300
350200
350100
350000
349900
349800
349700
349600
349500
349400
349300
349200
349100
349000

400

600

800

1000 1200

BH max

BH max
Poly. (BH
max)

0

500

y = -1.9714x2 + 3124.5x - 887889
1000 R² = 1 1500

c. BaFe12O19 + FeMn 5 wt%milling 15 menit.

B vs H

1000000

BH MAX

500000

Poly. (BH
MAX)
0
0

200

400

600

800

1000

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BH MAX

835000
820000
805000
790000
775000
760000
745000
730000
715000
700000
685000
670000
655000
640000
625000
610000
595000
580000
565000
550000
535000
520000
505000
490000
475000
460000
445000
430000
415000
400000
385000
370000
355000
340000
325000
310000

y = -10.65x2 + 12052x - 3E+06
R² = 1

BH MAX
Poly. (BH MAX)

0

200

400

600

800

1000

d. BaFe12O19 + FeMn 5 wt%milling 30 menit.

BH max

800000
600000
400000

BH max

200000

Poly. (BH
max)

0
0

200

400

600

800

1000

BH Max
640000
625000
610000
595000
580000
565000
550000
535000
520000
505000
490000
475000
460000
445000
430000
415000
400000
385000
370000
355000
340000
325000
310000

y = -5.0296x2 + 6905.9x - 2E+06
R² = 1

BH Max
Poly. (BH Max)

0

200

400

600

800

1000

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LAMPIRAN 8
DATA HASIL ANALISIS PSA ( Particle Size Analyzer )

1. Sampel Serbuk BaFe12O19

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88

2. Sampel Serbuk BaFe12O19 + 10 wt % FeMn milling 15 menit

Universitas Sumatera Utara

89

Universitas Sumatera Utara

90

3. Sampel Serbuk BaFe12O19 + 5 wt % FeMn milling 15 menit

Universitas Sumatera Utara

91

Universitas Sumatera Utara

92

4. Sampel Serbuk BaFe12O19 + 1 wt % FeMn milling 15 menit

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93

Universitas Sumatera Utara