Pengaruh Komposisi Dan Ketebalan Katoda LiMn2O4 (Lithium Mangan Oksida) Pada Kapasitas Baterai Ion Lithium
52
LAMPIRAN BAHAN
PVDF
LiMn2O4
Super P
DMAC
Universitas Sumatera Utara
53
LAMPIRAN ALAT
Neraca digital
Cawan
Al foil, Penggaris, Pisau
Beaker Glass
Penjepit dan Spatula
Pipet Tetes
Universitas Sumatera Utara
54
Oven
Doctor Blade
Mesin Press Hidrolik
Hot Plate dan Magnetic Stirrer
Oven Vakum
Glove Box
Universitas Sumatera Utara
55
Kaca Preparat
Oven
Holder
Jangka Sorong
Universitas Sumatera Utara
56
LAMPIRAN SAMPEL
Slurry (Lumpur)
Lembaran katoda ukuran 4x4 cm
Lembaran Katoda LiMn2O4
Lembaran katoda bentuk coin
Universitas Sumatera Utara
57
LAMPIRAN ALAT KARAKTERISASI
XRD
SEM
Optical Microscop (OM)
Alat Uji Charge Discharge
Universitas Sumatera Utara
58
Lampiran Perhitungan Massa LMO
Komposisi 85:10:5
Massa Al foil ukuran 4x4 cm = 0,07 gr
Massa Al foil ukuran coin cell = 0,0063 gr
Jari-jari dari coin cell = 0,725 cm
Luas coin cell = 1,65 cm2
Kode Sampel
85T1
85T2
85T3
Massa setelah dipress (4x4 cm) (gr)
0,15
0,17
0,18
Massa coin cell (gr)
0,0114
0,0178
0,0194
Kode Sampel ukuran 4x4 cm
LMO dalam laminate (gr/cm2)
LMO elektroda coin cell w(gr)
85T1
0,0068
= 0,00725
16
0,004335
85T2
0,085
= 0,00531
16
0,009775
85T3
0,011135
0,0935
= 0,00584
16
Komposisi 90:7:3
Massa Al foil ukuran 4x4 cm = 0,07 gr
Massa Al foil ukuran coin cell = 0,0063 gr
Jari-jari dari coin cell = 0,725 cm
Luas coin cell = 1,65 cm2
Kode Sampel
85T1
85T2
85T3
Massa setelah dipress (4x4 cm) (gr)
0,10
0,13
0,19
Massa coin cell (gr)
0,0105
0,0122
0,0186
Universitas Sumatera Utara
59
Kode Sampel ukuran 4x4 cm
LMO dalam laminate (gr/cm2)
LMO elektroda coin cell w(gr)
85T1
0,027
= 0,0016875
16
0,00378
85T2
0,054
= 0,003375
16
0,00531
85T3
0,01107
0,108
= 0,00675
16
Universitas Sumatera Utara
60
LAMPIRAN GRAFIK KAPASITAS DISCHARGE BATERAI
Sample: 85T1-10u
0.005mA, 3 – 4V
Universitas Sumatera Utara
61
Universitas Sumatera Utara
62
Sampel: 85T2-15u
0.005mA, 3 – 4V
Universitas Sumatera Utara
63
Universitas Sumatera Utara
64
Sampel 85T3-30u
0.005mA, 3 – 4V
Universitas Sumatera Utara
65
Universitas Sumatera Utara
66
Sampel 90T1-10u
0.005mA, 3 – 4 V
Universitas Sumatera Utara
67
Universitas Sumatera Utara
68
Sampel 90T2-15u
0.005mA, 3 – 4V
Universitas Sumatera Utara
69
Sampel 90T3-30u
0.005mA, 3 – 4V
Universitas Sumatera Utara
70
Universitas Sumatera Utara
71
Universitas Sumatera Utara
72
Analysis Results
General Information
Analysis date
2015/04/23 18:24:45
Sample name
LMO
Measurement date
2015/04/23 15:16:46
File name
LMO.ras
Operator
Ibrahim Purawiardi
Comment
Measurement profile
Universitas Sumatera Utara
73
Measurement conditions
X-Ray
40 kV , 30 mA
Scan speed / Duration time
3.0000 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
1/2deg
10.0mm
1/2deg
0.300mm
Universitas Sumatera Utara
74
Qualitative analysis results
Phase name
Formula
Figure of merit
Phase reg. detail
DB card number
Graphite-2H, syn
Lithium Manganese Oxide
C
Li Mn2 O4
0.310
1.393
ICDD (PDF-4+ 2013 RDB)
ICDD (PDF-4+ 2013 RDB)
00-056-0160
04-016-2988
Phase name
Formula
Space group
Phase reg. detail
DB card number
Graphite-2H, syn
Lithium Manganese Oxide
C
Li Mn2 O4
194 : P63/mmc
227 : Fd-3m,choice-2
ICDD (PDF-4+ 2013
ICDD (PDF-4+ 2013
00-056-0160
04-016-2988
Universitas Sumatera Utara
75
Meas. data:LMO/Data 1
Intensity (counts)
1.5e+004
1.0e+004
Integrated Intensity (counts deg)
5.0e+003
0.0e+000
8.0e+003
6.0e+003
4.0e+003
2.0e+003
0.0e+000
20
40
60
80
2-theta (deg)
Universitas Sumatera Utara
76
Peak list
No.
2-theta(deg)
d(ang.)
Height(counts)
FWHM(deg)
Int. I(counts deg)
Int. W(deg)
Asym. factor
1
2
3
4
5
6
7
8
9
10
11
12
13
18.9259
23.908(4)
26.5121(18)
27.535(10)
36.4832
42.36(3)
44.53(3)
50.73(12)
54.633(5)
59.67(2)
77.471(10)
83.537(16)
87.02(2)
4.68523
3.7189(6)
3.3593(2)
3.2368(11)
2.46082
2.1322(12)
2.0331(11)
1.798(4)
1.67854(15)
1.5483(5)
1.23105(13)
1.15639(18)
1.1189(2)
6.060307
114(11)
12383(111)
113(11)
11.943339
59(8)
90(9)
5(2)
395(20)
15(4)
84(9)
39(6)
31(6)
0.225891
0.185(15)
0.1834(13)
0.12(2)
0.225891
0.17(3)
0.52(4)
0.63(17)
0.226(7)
0.74(7)
0.156(8)
0.38(3)
0.25(3)
6.398392
30.6(12)
2974(9)
23.9(12)
4.530867
12.6(11)
84.9(18)
4.8(12)
127.5(13)
13.7(12)
17.4(6)
23.4(9)
11.0(7)
1.055787
0.27(4)
0.240(3)
0.21(3)
0.379363
0.22(5)
0.94(12)
0.9(6)
0.323(19)
0.9(3)
0.21(3)
0.60(12)
0.36(9)
1.58624
3.0(9)
2.10(10)
2.2(12)
1.58624
0.9(6)
1.3(4)
1.7(13)
2.2(3)
0.3(3)
0.8(2)
0.42(7)
1.6(8)
Universitas Sumatera Utara
77
Structure parameters
Data set name
Phase Name
Element
x
y
z
Occupancy
Temperature fa
LMO
LMO
LMO
LMO
LMO
Graphite-2H, syn
Graphite-2H, syn
Lithium Manganese
Lithium Manganese
Lithium Manganese
C
C
Li
Mn
O
0.000000
0.333333
0.125000
0.500000
0.244000
0.000000
0.666667
0.125000
0.500000
0.244000
0.250000
0.250000
0.125000
0.500000
0.244000
1.000
1.000
1.000
1.000
1.000
0.000
0.000
0.500
0.500
0.500
Data set name
Rwp
Rp
Re
S
Chi^2
Maximum shift/e.s.
LMO
13.3
8.3
9.58
1.3873
1.9247
0.076
Universitas Sumatera Utara
78
Lattice constants
Angular correction
Analysis results
Data set name
a(A)
b(A)
c(A)
alpha(deg)
beta(deg)
gamma(deg)
LMO
LMO
2.4613(10)
8.223(6)
2.4613(10)
8.223(6)
6.7173(5)
8.223(6)
90.000000
90.000000
90.000000
90.000000
120.000000
90.000000
Phase name
a(A)
b(A)
c(A)
alpha(deg)
beta(deg)
gamma(deg)
V(A^3)
Graphite-2H, syn
Lithium Manganese
2.4613(10)
8.223(6)
2.4613(10)
8.223(6)
6.7173(5)
8.223(6)
90.000000
90.000000
90.000000
90.000000
120.000000
90.000000
35.24(2)
556.1(7)
c
a
b
7.5
7
6.5
6
Lattice constants (ang.)
5.5
5
4.5
4
3.5
3
2.5
2
1.5
1
0.5
0
LMO
LMO
Data set
Universitas Sumatera Utara
79
Crystal structure analysis results
Indexing
Phase name
Formula
Figure of merit
Phase reg. detail
DB card number
Graphite-2H, syn
Lithium Manganese Oxide
C
Li Mn2 O4
0.310
1.393
ICDD (PDF-4+ 2013 RDB)
ICDD (PDF-4+ 2013 RDB)
00-056-0160
04-016-2988
Quantitative analysis results
-
Phase name
Content(%)
Graphite-2H, syn
Lithium Manganese Oxide
92.1(16)
7.9(5)
Lattice information
Phase name
a(A)
b(A)
c(A)
alpha(deg)
beta(deg)
gamma(deg)
V(A^3)
Graphite-2H, syn
Lithium Manganese
2.4613(10)
8.223(6)
2.4613(10)
8.223(6)
6.7173(5)
8.223(6)
90.000000
90.000000
90.000000
90.000000
120.000000
90.000000
35.24(2)
556.1(7)
Phase name
Space group
Z
Z'
Calc. density(g/cm^3)
Graphite-2H, syn
Lithium Manganese Oxide
194 : P63/mmc
227 : Fd-3m,choice-2
4
8
0.167
0.042
2.262
4.484
Structure determination
Refinement
Measurement range: 10.0000-90.0000deg Refinement range: 10.0000-90.0000deg (1.09 A), Rwp = 13.30% S = 1.3873
Phase name
Atomic coords
# of indep. reflns
Graphite-2H, syn
Lithium Manganese Oxide
Fractional coords
Fractional coords
11
19
Universitas Sumatera Utara
80
Universitas Sumatera Utara
81
Lampiran Perhitungan Kapasitas Discharge Secara Teori
•
Sampel: 85T1-10u
0,005mA, 3-4 V
I = 5 x 10-6 A
t = 2:27:42.1
= 2,56666667 Hr
C=Ixt
= 5 x 10-6 (2,56666667)
= 12,8333334 x 10-6
= 12,833 x 10-6 AHr
•
Sampel: 85T1-15u
0,005mA, 3-4 V
I = 5 x 10-6 A
t = 58:57.2
= 1,125 Hr
C=Ixt
= 5 x 10-6 (1,125)
= 5,625 x 10-6
= 5,625 x 10-6 AHr
•
Sampel: 85T1-30u
0,005mA, 3-4 V
I = 5 x 10-6 A
t = 1:15:16.0
= 1,29444444 Hr
C=Ixt
= 5 x 10-6 (1,29444444)
= 6,4722222 x 10-6
= 6,472 x 10-6 AHr
Universitas Sumatera Utara
82
•
Sampel: 90T1-10u
0,005mA, 3-4 V
I = 5 x 10-6 A
t = 2:45:35.0
= 2,8472222222 Hr
C=Ixt
= 5 x 10-6 (2,8472222222)
= 14,2361111111 x 10-6
= 12,236 x 10-6 AHr
•
Sampel: 90T1-15u
0,005mA, 3-4 V
-6
I = 5 x 10 A
t = 4:40:04.5
= 4,6777777778 Hr
C=Ixt
= 5 x 10-6 (4,6777777778)
= 23,3888888889 x 10-6
= 23,389 x 10-6 AHr
•
Sampel: 90T1-30u
0,005mA, 3-4 V
-6
I = 5 x 10 A
t = 50:55.6
= 0,9861111111 Hr
C=Ixt
= 5 x 10-6 (0,9861111111)
= 4,9305555555 x 10-6
= 4,931 x 10-6 AHr
Universitas Sumatera Utara
LAMPIRAN BAHAN
PVDF
LiMn2O4
Super P
DMAC
Universitas Sumatera Utara
53
LAMPIRAN ALAT
Neraca digital
Cawan
Al foil, Penggaris, Pisau
Beaker Glass
Penjepit dan Spatula
Pipet Tetes
Universitas Sumatera Utara
54
Oven
Doctor Blade
Mesin Press Hidrolik
Hot Plate dan Magnetic Stirrer
Oven Vakum
Glove Box
Universitas Sumatera Utara
55
Kaca Preparat
Oven
Holder
Jangka Sorong
Universitas Sumatera Utara
56
LAMPIRAN SAMPEL
Slurry (Lumpur)
Lembaran katoda ukuran 4x4 cm
Lembaran Katoda LiMn2O4
Lembaran katoda bentuk coin
Universitas Sumatera Utara
57
LAMPIRAN ALAT KARAKTERISASI
XRD
SEM
Optical Microscop (OM)
Alat Uji Charge Discharge
Universitas Sumatera Utara
58
Lampiran Perhitungan Massa LMO
Komposisi 85:10:5
Massa Al foil ukuran 4x4 cm = 0,07 gr
Massa Al foil ukuran coin cell = 0,0063 gr
Jari-jari dari coin cell = 0,725 cm
Luas coin cell = 1,65 cm2
Kode Sampel
85T1
85T2
85T3
Massa setelah dipress (4x4 cm) (gr)
0,15
0,17
0,18
Massa coin cell (gr)
0,0114
0,0178
0,0194
Kode Sampel ukuran 4x4 cm
LMO dalam laminate (gr/cm2)
LMO elektroda coin cell w(gr)
85T1
0,0068
= 0,00725
16
0,004335
85T2
0,085
= 0,00531
16
0,009775
85T3
0,011135
0,0935
= 0,00584
16
Komposisi 90:7:3
Massa Al foil ukuran 4x4 cm = 0,07 gr
Massa Al foil ukuran coin cell = 0,0063 gr
Jari-jari dari coin cell = 0,725 cm
Luas coin cell = 1,65 cm2
Kode Sampel
85T1
85T2
85T3
Massa setelah dipress (4x4 cm) (gr)
0,10
0,13
0,19
Massa coin cell (gr)
0,0105
0,0122
0,0186
Universitas Sumatera Utara
59
Kode Sampel ukuran 4x4 cm
LMO dalam laminate (gr/cm2)
LMO elektroda coin cell w(gr)
85T1
0,027
= 0,0016875
16
0,00378
85T2
0,054
= 0,003375
16
0,00531
85T3
0,01107
0,108
= 0,00675
16
Universitas Sumatera Utara
60
LAMPIRAN GRAFIK KAPASITAS DISCHARGE BATERAI
Sample: 85T1-10u
0.005mA, 3 – 4V
Universitas Sumatera Utara
61
Universitas Sumatera Utara
62
Sampel: 85T2-15u
0.005mA, 3 – 4V
Universitas Sumatera Utara
63
Universitas Sumatera Utara
64
Sampel 85T3-30u
0.005mA, 3 – 4V
Universitas Sumatera Utara
65
Universitas Sumatera Utara
66
Sampel 90T1-10u
0.005mA, 3 – 4 V
Universitas Sumatera Utara
67
Universitas Sumatera Utara
68
Sampel 90T2-15u
0.005mA, 3 – 4V
Universitas Sumatera Utara
69
Sampel 90T3-30u
0.005mA, 3 – 4V
Universitas Sumatera Utara
70
Universitas Sumatera Utara
71
Universitas Sumatera Utara
72
Analysis Results
General Information
Analysis date
2015/04/23 18:24:45
Sample name
LMO
Measurement date
2015/04/23 15:16:46
File name
LMO.ras
Operator
Ibrahim Purawiardi
Comment
Measurement profile
Universitas Sumatera Utara
73
Measurement conditions
X-Ray
40 kV , 30 mA
Scan speed / Duration time
3.0000 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
1/2deg
10.0mm
1/2deg
0.300mm
Universitas Sumatera Utara
74
Qualitative analysis results
Phase name
Formula
Figure of merit
Phase reg. detail
DB card number
Graphite-2H, syn
Lithium Manganese Oxide
C
Li Mn2 O4
0.310
1.393
ICDD (PDF-4+ 2013 RDB)
ICDD (PDF-4+ 2013 RDB)
00-056-0160
04-016-2988
Phase name
Formula
Space group
Phase reg. detail
DB card number
Graphite-2H, syn
Lithium Manganese Oxide
C
Li Mn2 O4
194 : P63/mmc
227 : Fd-3m,choice-2
ICDD (PDF-4+ 2013
ICDD (PDF-4+ 2013
00-056-0160
04-016-2988
Universitas Sumatera Utara
75
Meas. data:LMO/Data 1
Intensity (counts)
1.5e+004
1.0e+004
Integrated Intensity (counts deg)
5.0e+003
0.0e+000
8.0e+003
6.0e+003
4.0e+003
2.0e+003
0.0e+000
20
40
60
80
2-theta (deg)
Universitas Sumatera Utara
76
Peak list
No.
2-theta(deg)
d(ang.)
Height(counts)
FWHM(deg)
Int. I(counts deg)
Int. W(deg)
Asym. factor
1
2
3
4
5
6
7
8
9
10
11
12
13
18.9259
23.908(4)
26.5121(18)
27.535(10)
36.4832
42.36(3)
44.53(3)
50.73(12)
54.633(5)
59.67(2)
77.471(10)
83.537(16)
87.02(2)
4.68523
3.7189(6)
3.3593(2)
3.2368(11)
2.46082
2.1322(12)
2.0331(11)
1.798(4)
1.67854(15)
1.5483(5)
1.23105(13)
1.15639(18)
1.1189(2)
6.060307
114(11)
12383(111)
113(11)
11.943339
59(8)
90(9)
5(2)
395(20)
15(4)
84(9)
39(6)
31(6)
0.225891
0.185(15)
0.1834(13)
0.12(2)
0.225891
0.17(3)
0.52(4)
0.63(17)
0.226(7)
0.74(7)
0.156(8)
0.38(3)
0.25(3)
6.398392
30.6(12)
2974(9)
23.9(12)
4.530867
12.6(11)
84.9(18)
4.8(12)
127.5(13)
13.7(12)
17.4(6)
23.4(9)
11.0(7)
1.055787
0.27(4)
0.240(3)
0.21(3)
0.379363
0.22(5)
0.94(12)
0.9(6)
0.323(19)
0.9(3)
0.21(3)
0.60(12)
0.36(9)
1.58624
3.0(9)
2.10(10)
2.2(12)
1.58624
0.9(6)
1.3(4)
1.7(13)
2.2(3)
0.3(3)
0.8(2)
0.42(7)
1.6(8)
Universitas Sumatera Utara
77
Structure parameters
Data set name
Phase Name
Element
x
y
z
Occupancy
Temperature fa
LMO
LMO
LMO
LMO
LMO
Graphite-2H, syn
Graphite-2H, syn
Lithium Manganese
Lithium Manganese
Lithium Manganese
C
C
Li
Mn
O
0.000000
0.333333
0.125000
0.500000
0.244000
0.000000
0.666667
0.125000
0.500000
0.244000
0.250000
0.250000
0.125000
0.500000
0.244000
1.000
1.000
1.000
1.000
1.000
0.000
0.000
0.500
0.500
0.500
Data set name
Rwp
Rp
Re
S
Chi^2
Maximum shift/e.s.
LMO
13.3
8.3
9.58
1.3873
1.9247
0.076
Universitas Sumatera Utara
78
Lattice constants
Angular correction
Analysis results
Data set name
a(A)
b(A)
c(A)
alpha(deg)
beta(deg)
gamma(deg)
LMO
LMO
2.4613(10)
8.223(6)
2.4613(10)
8.223(6)
6.7173(5)
8.223(6)
90.000000
90.000000
90.000000
90.000000
120.000000
90.000000
Phase name
a(A)
b(A)
c(A)
alpha(deg)
beta(deg)
gamma(deg)
V(A^3)
Graphite-2H, syn
Lithium Manganese
2.4613(10)
8.223(6)
2.4613(10)
8.223(6)
6.7173(5)
8.223(6)
90.000000
90.000000
90.000000
90.000000
120.000000
90.000000
35.24(2)
556.1(7)
c
a
b
7.5
7
6.5
6
Lattice constants (ang.)
5.5
5
4.5
4
3.5
3
2.5
2
1.5
1
0.5
0
LMO
LMO
Data set
Universitas Sumatera Utara
79
Crystal structure analysis results
Indexing
Phase name
Formula
Figure of merit
Phase reg. detail
DB card number
Graphite-2H, syn
Lithium Manganese Oxide
C
Li Mn2 O4
0.310
1.393
ICDD (PDF-4+ 2013 RDB)
ICDD (PDF-4+ 2013 RDB)
00-056-0160
04-016-2988
Quantitative analysis results
-
Phase name
Content(%)
Graphite-2H, syn
Lithium Manganese Oxide
92.1(16)
7.9(5)
Lattice information
Phase name
a(A)
b(A)
c(A)
alpha(deg)
beta(deg)
gamma(deg)
V(A^3)
Graphite-2H, syn
Lithium Manganese
2.4613(10)
8.223(6)
2.4613(10)
8.223(6)
6.7173(5)
8.223(6)
90.000000
90.000000
90.000000
90.000000
120.000000
90.000000
35.24(2)
556.1(7)
Phase name
Space group
Z
Z'
Calc. density(g/cm^3)
Graphite-2H, syn
Lithium Manganese Oxide
194 : P63/mmc
227 : Fd-3m,choice-2
4
8
0.167
0.042
2.262
4.484
Structure determination
Refinement
Measurement range: 10.0000-90.0000deg Refinement range: 10.0000-90.0000deg (1.09 A), Rwp = 13.30% S = 1.3873
Phase name
Atomic coords
# of indep. reflns
Graphite-2H, syn
Lithium Manganese Oxide
Fractional coords
Fractional coords
11
19
Universitas Sumatera Utara
80
Universitas Sumatera Utara
81
Lampiran Perhitungan Kapasitas Discharge Secara Teori
•
Sampel: 85T1-10u
0,005mA, 3-4 V
I = 5 x 10-6 A
t = 2:27:42.1
= 2,56666667 Hr
C=Ixt
= 5 x 10-6 (2,56666667)
= 12,8333334 x 10-6
= 12,833 x 10-6 AHr
•
Sampel: 85T1-15u
0,005mA, 3-4 V
I = 5 x 10-6 A
t = 58:57.2
= 1,125 Hr
C=Ixt
= 5 x 10-6 (1,125)
= 5,625 x 10-6
= 5,625 x 10-6 AHr
•
Sampel: 85T1-30u
0,005mA, 3-4 V
I = 5 x 10-6 A
t = 1:15:16.0
= 1,29444444 Hr
C=Ixt
= 5 x 10-6 (1,29444444)
= 6,4722222 x 10-6
= 6,472 x 10-6 AHr
Universitas Sumatera Utara
82
•
Sampel: 90T1-10u
0,005mA, 3-4 V
I = 5 x 10-6 A
t = 2:45:35.0
= 2,8472222222 Hr
C=Ixt
= 5 x 10-6 (2,8472222222)
= 14,2361111111 x 10-6
= 12,236 x 10-6 AHr
•
Sampel: 90T1-15u
0,005mA, 3-4 V
-6
I = 5 x 10 A
t = 4:40:04.5
= 4,6777777778 Hr
C=Ixt
= 5 x 10-6 (4,6777777778)
= 23,3888888889 x 10-6
= 23,389 x 10-6 AHr
•
Sampel: 90T1-30u
0,005mA, 3-4 V
-6
I = 5 x 10 A
t = 50:55.6
= 0,9861111111 Hr
C=Ixt
= 5 x 10-6 (0,9861111111)
= 4,9305555555 x 10-6
= 4,931 x 10-6 AHr
Universitas Sumatera Utara