Sintesis Material Aktif Katoda LiFe0.9-xMnxNi0.1PO4 C Konsentrasi Mn 0 ≤ x≤ 0.2

42

LAMPIRAN A
BAHAN DAN PERALATAN

Lampiran A.1:Bahan yang dipakai pada pembuatan serbuk LiFeMnNiPO4/C

Serbuk LiOH.H2O

Serbuk MnO2

Larutan H3PO4

Serbuk Fe2O3

Serbuk Ni

Larutan Etanol

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Tepung Tapioka
Lampiran A.2 :Peralatan pada pembuatan serbuk LiFeMnNiPO4/C

Neraca Analitik

Ayakan 200 mesh

Mortar dan Pastel

Gelas Ukur

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Sendok dan spatula

Chamber dan Bola milling

Crucible

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High Temperature Furnace (46200)

Oven Pemanas

Alat Milling (SFM-1 Desk-Top Planetary

Alat XRD (X-Ray Diffraction)

Ball Miller)

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LAMPIRAN B
PROSES PEMBUATAN SERBUK LiFeMnNiPO4/C
Lampiran B.1 :Pembuatan Serbuk LiFeMnNiPO4/C

Serbuk LiOH.H2O

Serbuk MnO2

Bahan dicampur dengan larutan H3PO4

Serbuk Ni

Bahan dicampur dengan merata

Bahan dimasukkan kedalam Oven

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Bahan dihaluskan/digerus

Precursor sebelum dikalsinasi

Bahan diayak 200 mesh

Precursor sesudah dikalsinasi

Precursor sesudah dicampur dengan tepung tapioka

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LAMPIRAN C
PERHITUNGAN STOIKIOMETRI

Lampiran C.1 : Perhitungan Stoikiometri Kuantitatif (secara manual)
•

Target : 30 g LiFe0.7 Mn0.2 Ni0.1 PO4

•

Bahan Baku :
1. LiOH.H2O ( China / impor, 97,4 wt.%)
2. Fe2O3( Lokal / P2M2-LIPI, 96.25 wt.%)
3. MnO2( Lokal / P2M2-LIPI, 97.85 wt.%)

•

4. Ni

( Merck / Impor, 99.5 wt.% )

5. H3PO4

( China / Impor, 85 wt.% )

Ar / Mr
1. LiOH.H2O

= 41.962 g/mol

2. Fe2O3

= 159.687 g/mol

3. MnO2

= 86.936 g/mol

4. Ni

= 58.6934 g/mol

5. H3PO4

= 97.9938 g/mol

6. O2

= 31.998

g/mol

7. H2O

= 10.015

g/mol

8. LiFe0.7Mn0.2Ni0.1PO4 = 157.8582 g
•

Reaksi Target :
LiOH.H2O(s) + 0.35 Fe2O3(s) + 0.2 MnO2(s) + 0.1Ni(s) + H3PO4(l) →
LiFe0.7Mn0.2 Ni0.1 PO4(s) + 3H2O(g) + 0.225 O2(g)

•

n LiFe0.7 Mn0.2 Ni0.1 PO4

=
=

•

� ���� 0,7 � � 0,2 � �

0,1 �� 4 ������

�� ���� 0,7 � � 0,2 � �
30 �

0,1 �� 4

157.8582 �/���

= 0,1900 mol
Kebutuhan bahan baku / gas buang :

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=
•

��������� �� ℎ�� ���� ������ ℎ���

x n LiFe0.7 Mn0.2 Ni0.1 PO4 x Mr bahan

��������� ���� 0,7 � � 0,2 � �
0,1 �� 4

yang dibutuhkan

Kebutuhan bahan baku :

1. LiOH.H2O

=

2. Fe2O3

=

1

x 0,1900 mol x 41.962 g/mol

1

0,35
1

= 7.9727 g

x 0,1900 mol x 159.687 g/mol =10.6191

g
3. MnO3

=

4. Ni

=

5. H3PO4

=

0,2
1
0,1
1
1
1

x 0,1900 mol x 86.936 g/mol

= 3.3035 g

x 0,1900 mol x 58.6934 g/mol

= 1.1151g

x 0,1900 mol x 97.9938 g/mol

=18.6188g
__________+

•

41.6292g
Gas buang :
1. H2O

=

2. O2

=

3

x 0,1900 mol x 18.015 g/mol

1

0,225
1

= 10.2685 g

x 0,1900 mol x 31.998 g/mol = 1.3679 g
__________+

•

11.6364 g
Bahan – bahan yang harus di timbang :
1. LiOH.H2O

=

2. Fe2O3

=

3. MnO2

=

4. Ni

=

5. H3PO4

=

100 �� .%

97.4 �� .%

100 �� .%

x 7.9727 g

96.25 �� .%
100 �� .%

97.85 �� .%
100 �� .%

99.5 �� .%
100 �� .%
85 �� .%

= 8.18 g

x 10.6191 g = 11.03 g

x 3.3035 g

= 3.37 g

x 1.1151 g

= 1.12 g

x 18.6188 g

= 21.90 g

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Lampiran C.2 :Perhitungan Stoikiometri Kualitatif (secara manual)
Fasa
�-

Fe2

Sistem

SPGR

a(Ǻ)

b(Ǻ)

5.036 Ǻ

Rhombohe

R-3c

dral

(167)

Orthoromb

P2121

c(Ǻ)

�(°)

�(°)

�(°) Vol(Ǻ

Density(g/

)

cc)

5.036

5.426

62.35 62.3

60.

100.6

5.271g/cm

Ǻ

Ǻ

°

00°

2 Ǻ3

3

8.573(

8.690(

90.00 90.0

90.

622.9

3.195g/cm

00°

6Ǻ

3

109

256.7

3.063g/cm

.36

2 Ǻ3

3

5°

O3
LiFe

8.362(2

P3O9 ic

21(19) ) Ǻ

1) Ǻ

2) Ǻ

LiFe

P21(4) 4.8335(

8.101

6.9488 90.00 90.0

Monoclini

1) Ǻ

P2O7 c

4(2) Ǻ (5) Ǻ

°

0°

°

0°

3

°

Lampiran C.3 :Analisis Kuantitatif dengan Metode RIR
1.

Menetukan hkl [104]A dan [102]B

hkl [104]A→ 2� = 33,16600° → � = 16,583° Fe2O3

hkl [102]B→ 2� = 22,97590° → � = 11,487° LiFeP3O9
•

Dik : � = 16,583°

λ = 1,5406Ǻ = 0,15406 nm

maka :

sin �
�

- Fe →

- O→

=

sin 16,583
0,15406 ��

1,668−1

=

2−1
1,668−1
2−1

=

=

0,257
0,15406

�−23,68

20,05−23,68
�−7,245

5,623−7,245

= 1,668 nm-1

F = 21,25
F = 6,16

Maka F rata-rata = 13,705
•

F2 = 4F2 = 4 ( 13,705 )2 = 751,28
Dik : � = 11,487°

λ = 1,5406Ǻ = 0,15406 nm

maka :
-

sin �
�

=

Li →

sin 11,487
0,15406 ��

1,164−1
2−1

=

=

0,179
0,15406

�−2,215

1,742−2,215

= 1,164 nm-1
F = 2,13

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Fe →

-

O→

-

1,164−1

=

2−1
1,164−1
2−1

=

�−23,68

20,05−23,68
�−7,245

5,623−7,245

F = 23,08
F = 6,97

Maka F rata-rata = 10,72
F2 = F2 = (10,72)2 = 114,91
1. Untuk nilai P = 12 → hkl [104]A

Untuk nilai P = 24 → hkl [102]B

2. Menentukan LPF (Lorentz-Polarization Factor )
-

Untuk LPF hkl [104]A
16,583−16,5
16,6−16,5

-

=

���−22,02

21,74−22,02

Untuk LPF hkl [102]B
11,487−11,4

-

11,5−11,4

=

���−48,30

47,43−48,30

Maka :

→ LPF = 21,78
→ LPF = 47,54

R[104]A = F2 x P x LPF
= 751,28 x 12 x 21,78
= 196,35
R[102]B = F2 x P x LPF
= 114,91 x 24 x 47,54
= 131,107
3. Mencari fraksi volume (C)
��

��

=

��

��

=

x

��
��

99

10,2253

x

131,107
196,35

= 9,68 x 0,66
= 6,388
CA + CB = 1
6,388CB + CB = 1
7,388CB = 1
CB =

1
7,388

= 0,1353→ 13,53 wt.%

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CA + CB = 1
CA + 0,1353 = 1
CA = 1-0,1353
= 0,8647→ 86,47 wt.%
Misal :
mA :

0,8647 �/���
22,4 �

x Mr A

= 0,0386 x 159,69
= 6,164 gr

mB :

0,1353 �/���
22,4 �

x Mr A

= 0,00604 x 299,7
= 1,804 gr

mAB = 6,164 + 1,804
= 7,968 gr
4. Diubah ke ( wt.%)
-

mA ( wt.%) =
=

�� (�)

x 100%

��� (�� )
6,164

7,968

x 100%

= 0,773 x 100%
= 77,3 wt.%

-

mB ( wt.%) =
=

�� (�)

��� (�� )

1,804
7,968

x 100%

x 100%

= 0,226 x 100%
= 22,6 wt.%

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LAMPIRAN D
PENGAMATAN SEM

Lampiran D.1 : Pengamatan SEM Material Aktif LiFe0.7Mn0.2Ni0.1PO4/C

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Hasil mapping dari LiFe0.7Mn0.2Ni0.1PO4/C

Hasil SEM pada perbesaran 3000x

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Lampiran D.2 : Pengamatan SEM Material Aktif LiFe0.8Mn0.1Ni0.1PO4/C

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56

Hasil mapping dari LiFe0.8Mn0.1Ni0.1PO4/C

Hasil SEM dari LiFe0.8Mn0.1Ni0.1PO4/C

Lampiran D.3 : Pengamatan SEM Material Aktif LiFe0.9Ni0.1PO4/C

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Hasil mapping dari LiFe0.9Ni0.1PO4/C

Hasil SEM pada perbesaran 5000x

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LAMPIRAN E
PENGAMATAN XRD

Lampiran E.1 : Pengamatan XRD Material Aktif LiFe0.7Mn0.2Ni0.1PO4/C
04- 011- 4864

Feb 24, 2015 2

:40 PM (DELL)
Status Primary QM:Star Pressure/Temperature: Ambient Chemical Formula: FeP4O11
EmpiricalFormula: FeO11 P4 Weight%: Fe15.70O49.47 P34.83 Atomic%: Fe6.25O68.75P25.00
ANX: AB4X11 CompoundName: Iron PhosphorusOxide
d-Spacings
2θ
d( Å)
9.2774
9.524640
10.1883 8.675020
10.1883 8.675020
11.1545 7.925720
11.2472 7.860610
13.4675 6.569210
13.8474 6.389860
15.9489 5.552300
15.9489 5.552300
16.3123 5.429420
16.4438 5.386290
17.8551 4.963600
17.9739 4.931060
17.9739 4.931060
18.6164 4.762320
19.3099 4.592800
19.4153 4.568120
20.4583 4.337510
20.4583 4.337510
21.2965 4.168660
21.6869 4.094480
21.6869 4.094480
22.4164 3.962860
22.6045 3.930310
22.9528 3.871450
23.1423 3.840180
23.1423 3.840180
24.0733 3.693730
24.0733 3.693730
24.2218 3.671420
25.1073 3.543900
25.1073 3.543900
25.2362 3.526090
25.3281 3.513510
26.1717 3.402140
26.3113 3.384400
26.4191 3.370830
26.4191 3.370830
27.1258 3.284600
27.9822 3.185990
27.9822 3.185990
28.4818 3.131230
28.7097 3.106890
28.7097 3.106890
28.8031 3.097020
28.9761 3.078930
29.0807 3.068090
29.2073 3.055080
29.4580 3.029650
29.4580 3.029650
30.0621 2.970130
30.2738 2.949840
30.5085 2.927680
30.6457 2.914880
30.9493 2.886980
30.9493 2.886980
31.0343 2.879260
31.0343 2.879260
31.1695 2.867080
31.1695 2.867080
31.3008 2.855350
31.3008 2.855350
32.2177 2.776150
32.3606 2.764220
32.6093 2.743700
32.6093 2.743700
32.8538 2.723840

I
1
3m
m
3
3
1
11
5m
m
20
24
3
5m
m
14
95
88
139m
m
210
11m
m
999
925
98
105m
m
23m
m
40
137m
m
652
632
14
4
6m
m
26
83m
m
63
34m
m
22
22
10
4
10m
m
4
4
56
48
102m
m
159m
m
158m
m
218m
m
73
55
18m
m
9

h
0
1
-1
-1
-1
0
-2
1
1
0
0
-1
-1
-2
0
-2
-2
2
-2
2
1
-1
-2
-2
0
0
-3
1
-3
1
1
-2
2
2
-1
-1
-1
-1
0
-3
-4
-2
0
-2
0
-3
-3
2
3
3
-3
-3
-2
-2
3
4
1
-4
0
-4
2
-2
2
2
-1
-2
-2

k
0
1
1
1
-1
2
0
1
-1
2
-2
1
-1
0
0
2
-2
2
2
0
3
3
2
-2
2
-2
-1
1
1
-1
-3
0
2
-2
3
1
-1
-3
4
-1
0
2
4
-2
-4
3
-3
0
1
-1
3
-3
4
-4
3
0
-3
2
2
-2
4
4
2
-2
3
4
-4

l
1
0
0
1
1
0
1
1
1
1
1
2
2
2
2
1
1
0
0
1
0
0
2
2
2
2
2
2
0
2
1
3
1
1
2
3
3
2
0
3
2
3
1
3
1
1
1
2
1
1
2
2
1
1
0
0
2
2
3
2
0
0
2
2
3
2
2

*

2θ
32.9675
32.9675
33.1153
33.2391
33.2391
33.5336
33.8845
33.8845
34.1925
34.7094
34.7094
34.8114
34.8114
34.9889
34.9889
35.2392
35.2392
35.4110
35.4110
35.5591
36.3679
36.3679
36.7223
36.7223
36.8235
36.9118
37.1149
37.1149
37.2956
37.4749
37.7482
38.0155
38.0155
38.2855
38.4125
38.6830
38.8323
38.8323
38.9714
39.0615
39.2653
39.2653
39.4178
39.4178
39.6156
39.6156
39.7966
40.0818
40.0818
40.4916
40.4916
40.7020
40.8776
40.8776
41.1477
41.1477
41.2335
41.2335
41.6078
41.6078
42.2338
42.3990
42.3990
42.6550
42.6550
42.8334
42.8334

d( Å)
2.714710
2.714710
2.702930
2.693140
2.693140
2.670160
2.643310
2.643310
2.620200
2.582350
2.582350
2.575020
2.575020
2.562360
2.562360
2.544730
2.544730
2.532780
2.532780
2.522570
2.468300
2.468300
2.445290
2.445290
2.438800
2.433170
2.420320
2.420320
2.409010
2.397890
2.381160
2.365030
2.365030
2.348970
2.341490
2.325740
2.317140
2.317140
2.309190
2.304070
2.292580
2.292580
2.284060
2.284060
2.273110
2.273110
2.263190
2.247740
2.247740
2.225930
2.225930
2.214910
2.205800
2.205800
2.191940
2.191940
2.187580
2.187580
2.168760
2.168760
2.138050
2.130100
2.130100
2.117910
2.117910
2.109500
2.109500

I
24m
m
16
47m
m
4
132m
m
8
24m
m
17m
m
6m
m
13m
m
9m
m
19
65m
m
7m
m
10
9
40m
m
8
43
36
61m
m
4
5
23
24m
m
21
36
136m
m
102m
m
128m
m
11
11m
m
21m
m
13
16m
m
27m
m
27m
m
38m
m
5
33m
m
20m
m
19m
m

h
0
-1
1
0
1
-2
4
-4
-3
2
-3
2
-3
1
-1
3
-1
3
-1
-1
-2
-4
3
3
-5
-5
1
-2
1
-2
0
2
-1
-1
1
1
4
-4
4
-4
0
-4
-4
-4
0
-5
-3
-3
-3
-1
-5
-5
-3
-5
0
-3
-5
-5
4
-4
0
0
-6
1
-2
-1
-3

k
4
-3
1
-4
-1
0
2
2
-3
4
1
-4
-1
5
5
3
5
-3
1
-1
-2
0
1
-1
1
-1
5
4
-5
-4
0
0
5
-5
3
-3
2
2
-2
-2
4
4
-4
-4
-4
1
3
5
-3
3
-3
1
5
-1
6
-5
3
-3
4
4
6
-6
0
-1
0
5
1

l
2
3
3
2
3
4
0
0
3
1
4
1
4
0
0
1
1
1
4
4
4
4
2
2
3
3
1
3
1
3
4
3
2
2
3
3
1
4
1
4
3
1
1
2
3
0
4
1
4
4
2
4
2
4
0
2
1
1
0
0
1
1
3
4
5
3
5

*

2θ
43.4378
43.4378
43.5837
43.8615
43.8615
44.1942
44.1942
44.6145
44.7636
44.7636
45.0614
45.0614
45.4012
45.4012
45.5697
45.5697
45.7534
45.7534
46.0042
46.1543
46.4034
46.5276
46.7441
46.8973
46.8973
47.2000
47.2000
47.3025
47.3931
47.3931
47.5810
47.9603
48.7311
49.1820
49.1820
49.4158
49.4158
49.6984
49.6984
49.9192
50.0354
50.0354
50.4211
50.4211
50.5485
50.5485
50.8439
50.8439
50.9302
50.9302
51.0490
51.1994
51.1994
51.4079
51.4079
51.5555
51.5555
51.6918
51.6918
51.8128
51.8128
52.0124
52.0124
52.2016
52.2016

d( Å)
2.081540
2.081540
2.074910
2.062410
2.062410
2.047650
2.047650
2.029330
2.022920
2.022920
2.010240
2.010240
1.995980
1.995980
1.988990
1.988990
1.981430
1.981430
1.971210
1.965150
1.955180
1.950250
1.941720
1.935730
1.935730
1.924020
1.924020
1.920090
1.916630
1.916630
1.909500
1.895280
1.867090
1.851020
1.851020
1.842810
1.842810
1.832990
1.832990
1.825400
1.821430
1.821430
1.808400
1.808400
1.804140
1.804140
1.794350
1.794350
1.791510
1.791510
1.787620
1.782720
1.782720
1.775980
1.775980
1.771240
1.771240
1.766890
1.766890
1.763050
1.763050
1.756750
1.756750
1.750830
1.750830

I
13m
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8
14m
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48m
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11
9m
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11m
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16m
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8m
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49m
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5
14
12
4
5
14m
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14m
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12
16m
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3
4
9
29m
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30m
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60m
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18
11m
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38m
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17m
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17
13m
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10m
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10m
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24m
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46m
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38m
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13m
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Universitas Sumatera Utara