Pembuatan Baterai Lithium Menggunakan Bahan Aktif Mesocarbon Microbead (MCMB) Sebagai Anoda Dengan Variasi Persentase Berat Pelarut N,N-Dimethyl Acetamide (DMAC)
57
LAMPIRAN A
BAHAN DAN PERALATAN
A.1.1. Bahan yang Digunakan Pada Pembuatan Slurry
MCMB Kalsinasi 5000C
DMAC
MCMB Tanpa Perlakuan
PVDF
AB
Universitas Sumatera Utara
58
A.1.2 Bahan Yang DigunakanPada Pembuatan Baterai Prismatik
Cassing
Separator
Tab Anoda
Tab Katoda
A.2.1 Peralatan Pada Pembuatan Slurry
Beaker Glass & Sendok
Cawan Petri
Neraca Digital
Magnetik Stirerr
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59
Hot Plate
A.2.2 Peralatan Pada Pembuatan Lembaran
Docter Blade
Mesin Calendering
Oven Penyimpanan
Lembaran
Lembaran Kaca
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60
A.2.3 Peralatan Pada Assembly Baterai
Mesin Penyusun lembaran
Mesin Tabing
Mesin Penyusun lembaran
Mesin Tabing
Mesin Sealing
Glove Box
A.2.4 Peralatan Lainnya
Mikrometer
digital
Pisau, gunting, penggaris, spidol,
penjepit, kertas jeruk, pinset,
plastik sampel, kertas label,
masker, sarung tangan dan sendok.
Universitas Sumatera Utara
61
LAMPIRAN B
PEMBUATAN BATERAI LITHIUM PRISMATIK
B.1.1 Pembuatan Lembaran
B.2. Calendering Lembaran dan Pemotongan
B.2.1 Hasil Calendering
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62
B.2.2. Hasil Pemotongan
B.3. Assembly Baterai
Universitas Sumatera Utara
63
LAMPIRAN C
HASIL UJI SERBUK
LAMPIRAN C.1 : UJI XRD
C.1.1. Uji XRD Mesocarbon Microbead (MCMB) Tanpa kalsinasi
Universitas Sumatera Utara
64
Analysis Results
General Information
Analysis date
Sample name
File name
Comment
2015/02/17 13:42:09
MCMB non treat
MCMB non treat.ras
Measurement date
Operator
2015/02/17 13:20:05
Ibrahim Purawiardi
Measurement profile
5e+004
Intensity (cps)
4e+004
3e+004
2e+004
1e+004
Intensity (cps)
0e+000
5.0e+003
0.0e+000
-5.0e+003
20
40
60
80
2-theta (deg)
Universitas Sumatera Utara
65
Qualitative analysis results
Phase name
Graphite-2H
Formula
C
Figure of merit
0.281
Phase name
Graphite-2H
Formula
C
Space group
194 : P63/mmc
Phase reg. detail
ICDD (PDF-4+ 2013 RDB)
DB card number
00-041-1487
Phase reg. detail
ICDD (PDF-4+ 2013
RDB)
DB card number
00-041-1487
Universitas Sumatera Utara
66
Peak list
No.
1
2
3
4
5
6
7
2-theta(deg)
23.842(15)
26.451(4)
42.283(13)
44.639(11)
54.562(7)
59.94(19)
77.432(10)
d(ang.)
3.729(2)
3.3670(5)
2.1357(6)
2.0283(5)
1.6806(2)
1.542(4)
1.23157(14)
Height(cps)
278(48)
33035(525)
392(57)
382(56)
853(84)
42(19)
502(65)
FWHM(deg)
0.44(5)
0.226(3)
0.31(3)
1.00(3)
0.28(2)
1.17(17)
0.157(14)
Int. I(cps deg)
190(20)
10244(55)
214(11)
480(15)
386(7)
59(8)
134(4)
Int. W(deg)
0.68(19)
0.310(7)
0.55(11)
1.3(2)
0.45(5)
1.4(8)
0.27(4)
Asym. factor
1.9(9)
2.6(2)
0.23(5)
3.6(5)
3.3(4)
1.7(13)
0.5(2)
Universitas Sumatera Utara
67
Structure parameters
Data set name
MCMB non treat
MCMB non treat
Phase Name
Graphite-2H
Graphite-2H
Data set name
MCMB non treat
Rwp
20.15
Element
C
C
Rp
13.44
x
0.000000
0.333333
y
0.000000
0.666667
Re
14.78
z
0.250000
0.250000
S
1.3635
Occupancy
1.000
1.000
Chi^2
1.8591
Temperature factor
0.500
0.500
Maximum shift/e.s.d.
67
0.032
Universitas Sumatera Utara
68
Crystal structure analysis results
Indexing
Phase name
Graphite-2H
Formula
C
Figure of merit
0.281
Phase reg. detail
ICDD (PDF-4+ 2013 RDB)
DB card number
00-041-1487
Quantitative analysis results
Phase name
Graphite-2H
-
Content(%)
100.0(9)
Lattice information
Phase name
Graphite-2H
a(A)
2.4597(11)
Phase name
Graphite-2H
b(A)
2.4597(11)
c(A)
6.735(4)
Space group
194 : P63/mmc
alpha(deg)
90.000000
Z
4
beta(deg)
90.000000
gamma(deg)
120.000000
Z'
0.167
V(A^3)
35.29(3)
Calc. density(g/cm^3)
2.255
Structure determination
Refinement
Measurement range: 5.0000-80.0000deg Refinement range: 5.0000-80.0000deg (1.20 A)
Number of refined parameters: 31
Phase name
Atomic coords
Graphite-2H
Fractional coords
Rwp = 20.15% S = 1.3635
# of indep. reflns
8
Universitas Sumatera Utara
69
Universitas Sumatera Utara
70
C.1.2. Uji XRD Mesocarbon Microbead (MCMB) Kalsinasi 5000C
Universitas Sumatera Utara
71
Analysis Results
General Information
Analysis date
Sample name
File name
Comment
2015/04/21 11:49:46
MCMB T500
MCMB T500.ras
Measurement date
Operator
2015/04/21 11:11:38
Ibrahim Purawiardi
Measurement profile
5e+004
Meas. data:MCMB T500/Data 1
Calc. data:MCMB T500/Data 1
Error
Residual
Intensity (cps)
4e+004
3e+004
2e+004
1e+004
Intensity (cps)
0e+000
5.0e+003
0.0e+000
-5.0e+003
20
40
60
80
2-theta (deg)
Universitas Sumatera Utara
72
Qualitative analysis results
Phase name
Graphite-2H
Formula
C
Figure of merit
0.335
Phase name
Graphite-2H
Formula
C
Space group
194 : P63/mmc
Phase reg. detail
ICDD (PDF-4+ 2013 RDB)
DB card number
00-041-1487
Phase reg. detail
ICDD (PDF-4+ 2013
RDB)
DB card number
00-041-1487
Universitas Sumatera Utara
73
Peak list
No.
1
2
3
4
5
6
2-theta(deg)
26.4251(14)
42.326(13)
44.645(15)
54.531(8)
60.16(4)
77.462(10)
d(ang.)
3.37015(18)
2.1337(6)
2.0281(7)
1.6815(2)
1.5369(9)
1.23117(13)
Height(cps)
36064(425)
368(43)
407(45)
897(67)
53(16)
484(49)
FWHM(deg)
0.166(2)
0.33(2)
1.04(2)
0.265(14)
1.53(11)
0.162(12)
Int. I(cps deg)
9845(41)
224(9)
562(12)
401(6)
101(7)
126(3)
Int. W(deg)
0.273(4)
0.61(10)
1.38(18)
0.45(4)
1.9(7)
0.26(3)
Asym. factor
0.88(3)
0.36(7)
3.0(3)
1.12(14)
4(2)
0.9(3)
Universitas Sumatera Utara
74
Structure parameters
Data set name
MCMB T500
MCMB T500
Phase Name
Graphite-2H
Graphite-2H
Data set name
MCMB T500
Rwp
21.03
Element
C
C
Rp
13.73
x
0.000000
0.333333
y
0.000000
0.666667
Re
12.14
z
0.250000
0.250000
S
1.7323
Occupancy
1.000
1.000
Chi^2
3.0008
Temperature factor
0.500
0.500
Maximum shift/e.s.d.
0.038
Universitas Sumatera Utara
75
Crystal structure analysis results
Indexing
Phase name
Graphite-2H
Formula
C
Figure of merit
0.335
Phase reg. detail
ICDD (PDF-4+ 2013 RDB)
DB card number
00-041-1487
Quantitative analysis results
Phase name
Graphite-2H
-
Content(%)
100.0(10)
Lattice information
Phase name
Graphite-2H
a(A)
2.4674(4)
Phase name
Graphite-2H
b(A)
2.4674(4)
c(A)
6.7567(3)
Space group
194 : P63/mmc
alpha(deg)
90.000000
Z
4
beta(deg)
90.000000
gamma(deg)
120.000000
Z'
0.167
V(A^3)
35.624(9)
Calc. density(g/cm^3)
2.255
Structure determination
Refinement
Measurement range: 5.0000-90.0000deg Refinement range: 5.0000-90.0000deg (1.09 A)
Number of refined parameters: 31
Phase name
Atomic coords
Graphite-2H
Fractional coords
Rwp = 21.03% S = 1.73
# of indep. reflns
11
Universitas Sumatera Utara
76
Universitas Sumatera Utara
77
C.1.2 UJI SEM
C.1.2.1 MCMB Tanpa Kalsinasi
Hasil Image-J
Label
1
2
3
4
5
6
7
8
Mean
SD
Min
Max
Area
Mean
Min
Max
Angle
Length
153 139.399
101
252
0
152
109 138.578
92
224
0
108
121 157.991 127.733 239.800
1.909 120.067
43 164.279
131
213
0
42
106.500 150.062 112.933 232.200 0.477
105.517
46.228
13.046
19.374
17.182 0.955
46.235
43 138.578
92
213
0
42
153 164.279
131
252
1.909
152
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78
C.1.2.2 MCMB Kalsinasi 5000 C
Hasil Image-J
Label
1
2
3
4
5
6
7
Mean
SD
Min
Max
Area
Mean
Min
Max
Angle
Length
147 153.197
59
239
0
146
67 194.896
86 244.273
-1.736
66.030
139 135.591
62 252.304 0.830
138.014
117.667 161.228
69 245.192 -0.302
116.682
44.061
30.457
14.799
6.700
1.309
44.047
67 135.591
59
239
-1.736
66.030
147 194.896
86 252.304 0.830
146
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79
LAMPIRAN D
HASIL UJI PERFORMA BATERAI
LAMPIRAN D.1. : UJI CHARGE-DISCHARGE BATERAI
D.1.1. Charge-discharge Sampel A
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80
D.1.2. Uji Charge-discharge Sampel B
Universitas Sumatera Utara
81
D.1.3. Uji Charge-discharge Sampel C
Universitas Sumatera Utara
82
C.1.4 Uji Charge-Discharge Sampel D
Universitas Sumatera Utara
83
D.2 Uji Cyclic Voltammetri
D.2.1. CV Sampel A
D.2.2 CV Sampel B
Universitas Sumatera Utara
84
D.2.3 CV Sampel C
D.2.4 CV Sampel D
Universitas Sumatera Utara
85
LAMPIRAN E
PERHITUNGAN KOMPOSISI SAMPEL DAN ANALISA
E.1. Perhitungan Komposisi Sampel
1.
Perbandingan bahan baku pada saat pembuatan sampel :
2.
Material aktif : PVDF : AB = 85 : 10 : 5
MCMB : 3 g (85%)
PVDF :
AB
:
Perbandingan MCMB terhadap pelarut DMAC :
MCMB : DMAC = 3 : 7
Persentase berat DMAC =
MCMB : DMAC = 3 : 9
Persentase berat DMAC =
MCMB : DMAC = 3 : 11
Persentase berat DMAC =
E.2. Perhitungan Analisa
1.
Efisiensi dari Anoda MCMB
η=
Dimana :
η
= Efisiensi (%)
= Kapasitas discharge anoda (mAh)
= Kapasitas charge anoda (mAh)
Efisiensi pada baterai sampel B, dengan pelarut DMAC 33,33 %
η=
η=
Universitas Sumatera Utara
86
2.
Kapasitas spesifik MCMB
Cspesifik =
Dimana :
Cspesifik = kapasitas spesifik (mAh/g)
Cd
= Kapasitas discharge (mAh)
m
= Massa MCMB (g)
Kapasitas spesifik pada baterai sampel D, anoda dengan serbuk MCMB
tanpa kalsinasi dan 33,33% berat pelarut DMAC.
Cspesifik =
Cspesifik =
= 20,12 mAh/g
Universitas Sumatera Utara
LAMPIRAN A
BAHAN DAN PERALATAN
A.1.1. Bahan yang Digunakan Pada Pembuatan Slurry
MCMB Kalsinasi 5000C
DMAC
MCMB Tanpa Perlakuan
PVDF
AB
Universitas Sumatera Utara
58
A.1.2 Bahan Yang DigunakanPada Pembuatan Baterai Prismatik
Cassing
Separator
Tab Anoda
Tab Katoda
A.2.1 Peralatan Pada Pembuatan Slurry
Beaker Glass & Sendok
Cawan Petri
Neraca Digital
Magnetik Stirerr
Universitas Sumatera Utara
59
Hot Plate
A.2.2 Peralatan Pada Pembuatan Lembaran
Docter Blade
Mesin Calendering
Oven Penyimpanan
Lembaran
Lembaran Kaca
Universitas Sumatera Utara
60
A.2.3 Peralatan Pada Assembly Baterai
Mesin Penyusun lembaran
Mesin Tabing
Mesin Penyusun lembaran
Mesin Tabing
Mesin Sealing
Glove Box
A.2.4 Peralatan Lainnya
Mikrometer
digital
Pisau, gunting, penggaris, spidol,
penjepit, kertas jeruk, pinset,
plastik sampel, kertas label,
masker, sarung tangan dan sendok.
Universitas Sumatera Utara
61
LAMPIRAN B
PEMBUATAN BATERAI LITHIUM PRISMATIK
B.1.1 Pembuatan Lembaran
B.2. Calendering Lembaran dan Pemotongan
B.2.1 Hasil Calendering
Universitas Sumatera Utara
62
B.2.2. Hasil Pemotongan
B.3. Assembly Baterai
Universitas Sumatera Utara
63
LAMPIRAN C
HASIL UJI SERBUK
LAMPIRAN C.1 : UJI XRD
C.1.1. Uji XRD Mesocarbon Microbead (MCMB) Tanpa kalsinasi
Universitas Sumatera Utara
64
Analysis Results
General Information
Analysis date
Sample name
File name
Comment
2015/02/17 13:42:09
MCMB non treat
MCMB non treat.ras
Measurement date
Operator
2015/02/17 13:20:05
Ibrahim Purawiardi
Measurement profile
5e+004
Intensity (cps)
4e+004
3e+004
2e+004
1e+004
Intensity (cps)
0e+000
5.0e+003
0.0e+000
-5.0e+003
20
40
60
80
2-theta (deg)
Universitas Sumatera Utara
65
Qualitative analysis results
Phase name
Graphite-2H
Formula
C
Figure of merit
0.281
Phase name
Graphite-2H
Formula
C
Space group
194 : P63/mmc
Phase reg. detail
ICDD (PDF-4+ 2013 RDB)
DB card number
00-041-1487
Phase reg. detail
ICDD (PDF-4+ 2013
RDB)
DB card number
00-041-1487
Universitas Sumatera Utara
66
Peak list
No.
1
2
3
4
5
6
7
2-theta(deg)
23.842(15)
26.451(4)
42.283(13)
44.639(11)
54.562(7)
59.94(19)
77.432(10)
d(ang.)
3.729(2)
3.3670(5)
2.1357(6)
2.0283(5)
1.6806(2)
1.542(4)
1.23157(14)
Height(cps)
278(48)
33035(525)
392(57)
382(56)
853(84)
42(19)
502(65)
FWHM(deg)
0.44(5)
0.226(3)
0.31(3)
1.00(3)
0.28(2)
1.17(17)
0.157(14)
Int. I(cps deg)
190(20)
10244(55)
214(11)
480(15)
386(7)
59(8)
134(4)
Int. W(deg)
0.68(19)
0.310(7)
0.55(11)
1.3(2)
0.45(5)
1.4(8)
0.27(4)
Asym. factor
1.9(9)
2.6(2)
0.23(5)
3.6(5)
3.3(4)
1.7(13)
0.5(2)
Universitas Sumatera Utara
67
Structure parameters
Data set name
MCMB non treat
MCMB non treat
Phase Name
Graphite-2H
Graphite-2H
Data set name
MCMB non treat
Rwp
20.15
Element
C
C
Rp
13.44
x
0.000000
0.333333
y
0.000000
0.666667
Re
14.78
z
0.250000
0.250000
S
1.3635
Occupancy
1.000
1.000
Chi^2
1.8591
Temperature factor
0.500
0.500
Maximum shift/e.s.d.
67
0.032
Universitas Sumatera Utara
68
Crystal structure analysis results
Indexing
Phase name
Graphite-2H
Formula
C
Figure of merit
0.281
Phase reg. detail
ICDD (PDF-4+ 2013 RDB)
DB card number
00-041-1487
Quantitative analysis results
Phase name
Graphite-2H
-
Content(%)
100.0(9)
Lattice information
Phase name
Graphite-2H
a(A)
2.4597(11)
Phase name
Graphite-2H
b(A)
2.4597(11)
c(A)
6.735(4)
Space group
194 : P63/mmc
alpha(deg)
90.000000
Z
4
beta(deg)
90.000000
gamma(deg)
120.000000
Z'
0.167
V(A^3)
35.29(3)
Calc. density(g/cm^3)
2.255
Structure determination
Refinement
Measurement range: 5.0000-80.0000deg Refinement range: 5.0000-80.0000deg (1.20 A)
Number of refined parameters: 31
Phase name
Atomic coords
Graphite-2H
Fractional coords
Rwp = 20.15% S = 1.3635
# of indep. reflns
8
Universitas Sumatera Utara
69
Universitas Sumatera Utara
70
C.1.2. Uji XRD Mesocarbon Microbead (MCMB) Kalsinasi 5000C
Universitas Sumatera Utara
71
Analysis Results
General Information
Analysis date
Sample name
File name
Comment
2015/04/21 11:49:46
MCMB T500
MCMB T500.ras
Measurement date
Operator
2015/04/21 11:11:38
Ibrahim Purawiardi
Measurement profile
5e+004
Meas. data:MCMB T500/Data 1
Calc. data:MCMB T500/Data 1
Error
Residual
Intensity (cps)
4e+004
3e+004
2e+004
1e+004
Intensity (cps)
0e+000
5.0e+003
0.0e+000
-5.0e+003
20
40
60
80
2-theta (deg)
Universitas Sumatera Utara
72
Qualitative analysis results
Phase name
Graphite-2H
Formula
C
Figure of merit
0.335
Phase name
Graphite-2H
Formula
C
Space group
194 : P63/mmc
Phase reg. detail
ICDD (PDF-4+ 2013 RDB)
DB card number
00-041-1487
Phase reg. detail
ICDD (PDF-4+ 2013
RDB)
DB card number
00-041-1487
Universitas Sumatera Utara
73
Peak list
No.
1
2
3
4
5
6
2-theta(deg)
26.4251(14)
42.326(13)
44.645(15)
54.531(8)
60.16(4)
77.462(10)
d(ang.)
3.37015(18)
2.1337(6)
2.0281(7)
1.6815(2)
1.5369(9)
1.23117(13)
Height(cps)
36064(425)
368(43)
407(45)
897(67)
53(16)
484(49)
FWHM(deg)
0.166(2)
0.33(2)
1.04(2)
0.265(14)
1.53(11)
0.162(12)
Int. I(cps deg)
9845(41)
224(9)
562(12)
401(6)
101(7)
126(3)
Int. W(deg)
0.273(4)
0.61(10)
1.38(18)
0.45(4)
1.9(7)
0.26(3)
Asym. factor
0.88(3)
0.36(7)
3.0(3)
1.12(14)
4(2)
0.9(3)
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74
Structure parameters
Data set name
MCMB T500
MCMB T500
Phase Name
Graphite-2H
Graphite-2H
Data set name
MCMB T500
Rwp
21.03
Element
C
C
Rp
13.73
x
0.000000
0.333333
y
0.000000
0.666667
Re
12.14
z
0.250000
0.250000
S
1.7323
Occupancy
1.000
1.000
Chi^2
3.0008
Temperature factor
0.500
0.500
Maximum shift/e.s.d.
0.038
Universitas Sumatera Utara
75
Crystal structure analysis results
Indexing
Phase name
Graphite-2H
Formula
C
Figure of merit
0.335
Phase reg. detail
ICDD (PDF-4+ 2013 RDB)
DB card number
00-041-1487
Quantitative analysis results
Phase name
Graphite-2H
-
Content(%)
100.0(10)
Lattice information
Phase name
Graphite-2H
a(A)
2.4674(4)
Phase name
Graphite-2H
b(A)
2.4674(4)
c(A)
6.7567(3)
Space group
194 : P63/mmc
alpha(deg)
90.000000
Z
4
beta(deg)
90.000000
gamma(deg)
120.000000
Z'
0.167
V(A^3)
35.624(9)
Calc. density(g/cm^3)
2.255
Structure determination
Refinement
Measurement range: 5.0000-90.0000deg Refinement range: 5.0000-90.0000deg (1.09 A)
Number of refined parameters: 31
Phase name
Atomic coords
Graphite-2H
Fractional coords
Rwp = 21.03% S = 1.73
# of indep. reflns
11
Universitas Sumatera Utara
76
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C.1.2 UJI SEM
C.1.2.1 MCMB Tanpa Kalsinasi
Hasil Image-J
Label
1
2
3
4
5
6
7
8
Mean
SD
Min
Max
Area
Mean
Min
Max
Angle
Length
153 139.399
101
252
0
152
109 138.578
92
224
0
108
121 157.991 127.733 239.800
1.909 120.067
43 164.279
131
213
0
42
106.500 150.062 112.933 232.200 0.477
105.517
46.228
13.046
19.374
17.182 0.955
46.235
43 138.578
92
213
0
42
153 164.279
131
252
1.909
152
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C.1.2.2 MCMB Kalsinasi 5000 C
Hasil Image-J
Label
1
2
3
4
5
6
7
Mean
SD
Min
Max
Area
Mean
Min
Max
Angle
Length
147 153.197
59
239
0
146
67 194.896
86 244.273
-1.736
66.030
139 135.591
62 252.304 0.830
138.014
117.667 161.228
69 245.192 -0.302
116.682
44.061
30.457
14.799
6.700
1.309
44.047
67 135.591
59
239
-1.736
66.030
147 194.896
86 252.304 0.830
146
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LAMPIRAN D
HASIL UJI PERFORMA BATERAI
LAMPIRAN D.1. : UJI CHARGE-DISCHARGE BATERAI
D.1.1. Charge-discharge Sampel A
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D.1.2. Uji Charge-discharge Sampel B
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D.1.3. Uji Charge-discharge Sampel C
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C.1.4 Uji Charge-Discharge Sampel D
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D.2 Uji Cyclic Voltammetri
D.2.1. CV Sampel A
D.2.2 CV Sampel B
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D.2.3 CV Sampel C
D.2.4 CV Sampel D
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LAMPIRAN E
PERHITUNGAN KOMPOSISI SAMPEL DAN ANALISA
E.1. Perhitungan Komposisi Sampel
1.
Perbandingan bahan baku pada saat pembuatan sampel :
2.
Material aktif : PVDF : AB = 85 : 10 : 5
MCMB : 3 g (85%)
PVDF :
AB
:
Perbandingan MCMB terhadap pelarut DMAC :
MCMB : DMAC = 3 : 7
Persentase berat DMAC =
MCMB : DMAC = 3 : 9
Persentase berat DMAC =
MCMB : DMAC = 3 : 11
Persentase berat DMAC =
E.2. Perhitungan Analisa
1.
Efisiensi dari Anoda MCMB
η=
Dimana :
η
= Efisiensi (%)
= Kapasitas discharge anoda (mAh)
= Kapasitas charge anoda (mAh)
Efisiensi pada baterai sampel B, dengan pelarut DMAC 33,33 %
η=
η=
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2.
Kapasitas spesifik MCMB
Cspesifik =
Dimana :
Cspesifik = kapasitas spesifik (mAh/g)
Cd
= Kapasitas discharge (mAh)
m
= Massa MCMB (g)
Kapasitas spesifik pada baterai sampel D, anoda dengan serbuk MCMB
tanpa kalsinasi dan 33,33% berat pelarut DMAC.
Cspesifik =
Cspesifik =
= 20,12 mAh/g
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