1. PERHITUNGAN PENCAMPURAN BAHAN BAHAN 1.1 Menghitung massa bahan LTO - Studi TiO2 Sebagai Bahan Pembentukan Elektroda Anoda Berbasis Titanate Dalam Aplikasi Pada Baterai Ion Lithium
LAMPIRAN A
1. PERHITUNGAN PENCAMPURAN BAHAN BAHAN
1.1 Menghitung massa bahan LTO
4LiOH.H2O + 5TiO2
Li4Ti5O12 + 3H2O
Massa atom relatif unsur :
Li = 7
Ti = 47,867
O = 15,9994
Mr LiOH.H2O
TiO2
= 41,9988
= 79,8658
Li4Ti5O12
•
= 459,3278
massa LiOH .H 2 O
1 x Mr LiOH .H 2 O
=
Massa LiOH.H2O =
=
20 gr
Mr Li 4 Ti 5 O 12
1 x Mr LiOH .H 2 O
Mr Li 4 Ti 5 O 12
1 𝑥𝑥41,9988 x 20 gr
459,3278
= 1,828707 gr
•
massa Ti O 2
1 x Mr Ti O 2
=
Massa TiO2
=
=
20 gr
Mr Li 4 Ti 5 O 12
1 x Mr Ti O 2 x 20 gr
Mr Li 4 Ti 5 O 12
1 x 79,8658 x 20 gr
459,3278
= 3,47750 gr
1.2.Menghitung massa bahan NaLiTi3O7
LiOH.H2O + 3 TiO2 + ½ Na2CO3
NaLiTi3O7 + ½ CO2 + ½ H2O + H2
Massa atom relatif unsur :
Universitas Sumatera Utara
Na = 22,989
Li = 7
Ti = 47,867
C = 12,0107
O = 15,9994
Mr LiOH.H2O = 41,9988
TiO2
= 79,8658
Na2CO3
= 105,9707
NaLiTi3O7 = 285,548
•
massa LiOH .H 2 O
1 x Mr LiOH .H 2 O
=
Massa LiOH.H2O =
=
10 gr
Mr NaLi Ti 3 O 7
1 x Mr LiOH .H 2 O x 10 gr
Mr NaLi Ti 3 O 7
1 𝑥𝑥41,9988 x 10 gr
285,548
= 1,470814 gr
•
massa Ti O 2
1 x Mr Ti O 2
=
Massa TiO2
=
=
10 gr
Mr NaLi Ti 3 O 7
1 x Mr Ti O 2 x 10 gr
Mr NaLi Ti 3 O 7
1 x 79,8658 x 10 gr
285,548
= 8,3907924 gr
•
massa Na 2 CO 3
1 x Mr Na 2 O 3
Massa Na2CO3
=
=
=
10 gr
Mr NaLi Ti 3 O 7
1 x Mr Na 2 O 3 x 10 gr
Mr NaLi Ti 3 O 7
1 x 105,9707 x 10 gr
285,548
= 1,470814 gr
Universitas Sumatera Utara
2. MENGHITUNG SPECIFIC CAPACITY TiO2
Li + TiO2 + e-
LixTiO2
Berat atom Ti = 47,867
Berat atom O = 15,999
Berat atom TiO2 = 47,867 + 2(15,999)
= 79,856 x 10-3
Specific capacity = (N x F ) / (berat atom)
Dimana : N= valensi atom
F = Konstanta Faraday (96485 colomb/mol) (26,801 Ah/mol)
Specific capacity = (1 x 26,801) / (79,865 x 10-3)
= 335,57 mAh/g
3. MENGUKUR KETEBALAN SAMPEL Li4Ti5O12 DAN NaLiTi3O12
Tebal Cu foil : 10 чm
Sampel
L (чm)
TiO2
Li4Ti5O12
NaLiTi3O12
60
90
70
L – Cu
Foil
50
80
60
Rs (Ω)
36,4
72,5
21,3
Mengukur konduktivitas
L0 = 50 x 10-6 m
L1 = 80 x 10-6 m
L2 = 70 x 10-6 m
R1 = 36,4 Ω
R1 = 72,5 Ω
R2 = 21,3 Ω
A = 5,77 mm
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Na-0 => R = ρ
L
A
50 x 10 −6 m
36,4 Ω = ρ
5,77 x 1,67 x 10 −6 m 2
50 m
36,4 Ω = ρ
5,77 x 1,67 m
ρ = 7,014 Ωm = 701,4 Ωcm
σ =
1
𝜌𝜌
1
= 701,4 Ωcm
= 0,001425 S/cm
Na-1 => R = ρ
L
A
80 x 10 −6 m
72,5 Ω = ρ
72,5 Ω = ρ
5,77 x 1,67 x 10 −6 m 2
80 m
5,77 x 1,67 m
ρ = 8,732 Ωm = 873,2 Ωcm
σ =
1
𝜌𝜌
1
= 873,2 Ωcm
= 0,00114 S/cm
Na-2 => R = ρ
L
A
21,3 Ω = ρ
21,3 Ω = ρ
70 x 10 −6 m
5,77 x 1,67 x 10 −6 m 2
70 m
5,77 x 1,67 m
ρ = 0,2932 Ωm = 293,2 Ωcm
σ =
1
𝜌𝜌
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1
= 293,2 Ωcm
= 0,00341 S/cm
4. MENGHITUNG MASSA JENIS PADA SAMPEL
Volume kosong : 43,3389 gr
Volume garis = 0,7439 cm3
Serbuk
Na0
Na1
Na2
Gr
43,8859
43,9349
43,9856
Netto
0,547
0,596
0,6467
ρSerbuk
0,7353
0,801
0,8693
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LAMPIRAN B
1.Gambar Peralatan
Beaker glass
Spatula
Beaker glass
Pipet tetes
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Penjepit
Wadah
Magnetic stirer
Ayakan
Wadah
Mortar
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Oven
Hot Plate
Oven dan Doctor Blade
Neraca digital
furnace
Pisau Doctor Blade
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Thickness gaoge
Glove box
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2. Gambar Bahan
LiOH.H2O
Na2CO3
PVDF
TiO2
DMAC
Separator
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Lithium metal
Cu foil
GAMBAR LEMBARAN
Lembaran Na0
Lembaran Na1
Lembaran Na2
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3. Gambar Alat Karaterisasi Dan Uji
Scanning Electron Microscopy (SEM)
X-Ray diffraction (XRD)
Cyclic Voltammetry dan Charge discharge
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Lampiran C
Hasil xrd TiO2, Li4Ti5O12, dan NaLiTi3O7
1. Sampel Na0
Meas. data:TiO2 china/Data 1
Calc. data:TiO2 china/Data 1
Error
Residual
Intensity (counts)
800
600
400
200
Intensity (counts)
0
100
0
-100
20
40
60
80
2-theta (deg)
Peak list
No.
2theta(deg)
d(ang.)
Height(count
s)
FWHM(deg)
Int. I(counts
deg)
Int. W(deg)
Asym. factor
1
25.284(6)
3.5196(8)
572(24)
0.134(4)
97.4(15)
0.170(10)
1.4(3)
2
36.949(7)
2.4309(4)
31(6)
0.117(17)
5.1(4)
0.16(4)
3(2)
3
37.788(8)
2.3788(5)
101(10)
0.150(9)
19.1(5)
0.19(2)
1.9(5)
4
38.555(14)
2.3332(8)
37(6)
0.120(16)
5.6(3)
0.15(3)
0.8(4)
5
48.015(6)
1.8933(2)
171(13)
0.117(6)
27.3(6)
0.159(16)
0.73(17)
6
53.847(5)
1.70118(15)
99(10)
0.122(9)
17.2(6)
0.17(2)
0.45(6)
7
55.067(7)
1.6663(2)
103(10)
0.112(9)
17.9(5)
0.17(2)
1.9(6)
8
62.13(3)
1.4929(7)
14(4)
0.19(3)
3.0(3)
0.22(9)
2.1(19)
9
62.669(11)
1.4812(2)
78(9)
0.120(9)
13.3(5)
0.17(3)
1.0(4)
10
68.745(16)
1.3644(3)
33(6)
0.142(14)
5.9(4)
0.18(4)
1.2(6)
11
70.261(11)
1.33862(18)
31(6)
0.159(15)
5.9(4)
0.19(5)
0.52(16)
12
75.067(16)
1.2644(2)
45(7)
0.167(13)
9.3(5)
0.21(4)
2.3(11)
13
76.03(3)
1.2508(4)
16(4)
0.144(19)
2.7(3)
0.17(6)
1.4(11)
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14
82.68(3)
1.1662(3)
22(5)
0.17(3)
5.3(5)
0.24(7)
1.3(10)
15
83.14(3)
1.1609(4)
10(3)
0.19(4)
2.5(4)
0.26(12)
0.7(6)
Qualitative analysis results
Phase name
Formula
Figure of merit
Phase reg. detail
DB card number
anatase, nano
Ti O2
0.144
ICDD (PDF-4+ 2014 RDB)
00-064-0863
Phase name
Formula
Space group
Phase reg. detail
DB card number
anatase, nano
Ti O2
141 : I41/amd,choice-2
ICDD (PDF-4+ 2014 RDB)
00-064-0863
Universitas Sumatera Utara
Dik : Fwhm = 0,134o
B = 3,722 x 10-4 rad
2θ = 25,284 0
θ= 12, 642
cos θ = 0,9750
λ = 1,54060 x 10-10m
k = 0,94
dit : ukuran partikel (d)= ...?
penyelesaian :
ukuran kristal (d) =
𝑘𝑘 λ
B cos θ
0,94 𝑥𝑥 1,54060 𝑥𝑥 10 −10
d = 3,722 x
=
10 −4 rad .0,975 0
1,448164 𝑥𝑥 10 −10
3,62895 x 10 −4
= 0,3990x 10-6
= 0,3990 чm
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2. Sampel Na1
Meas. data:LTO/Data 1
Calc. data:LTO/Data 1
Error
Residual
Intensity (counts)
Intensity (counts)
600
400
200
0
100
50
0
-50
-100
20
40
60
80
2-theta (deg)
Peak list
No.
2-theta(deg)
d(ang.)
Height(coun
ts)
FWHM(
deg)
Int. I(counts deg)
Int. W(deg)
Asym. factor
1
21.326(14)
4.163(3)
14(4)
0.16(4)
2.9(4)
0.21(9)
0.6(9)
2
25.304(6)
3.5169(9)
540(23)
0.130(4
90.6(14)
0.168(10)
1.5(3)
3
30.58(5)
2.921(5)
12(3)
0.25(4)
3.5(5)
0.29(12)
1.0(8)
4
31.71(4)
2.820(4)
13(4)
0.34(3)
4.6(5)
0.36(14)
0.7(3)
5
36.94(2)
2.4316(13)
36(6)
0.13(2)
6.1(4)
0.17(4)
0.9(6)
6
37.804(10)
2.3778(6)
104(10)
0.133(1
17.6(7)
0.17(2)
2.2(9)
7
38.56(3)
2.3328(16)
31(6)
0.16(2)
5.7(4)
0.19(5)
0.8(5)
8
48.048(7)
1.8920(3)
150(12)
0.134(8
26.1(7)
0.174(19)
1.4(3)
9
53.901(11)
1.6996(3)
81(9)
0.159(1
17.1(6)
0.21(3)
1.8(7)
10
55.067(9)
1.6663(2)
101(10)
0.116(8
16.0(5)
0.16(2)
1.5(5)
11
62.142(7)
1.49253(1
17(4)
0.13(2)
3.1(3)
0.18(6)
5(4)
12
62.687(10)
1.4809(2)
68(8)
0.135(1
11.7(5)
0.17(3)
0.9(3)
13
68.74(2)
1.3644(3)
26(5)
0.18(2)
6.0(4)
0.23(6)
0.7(3)
14
70.321(8)
1.33762(1
31(6)
0.150(1
6.0(3)
0.20(5)
2.6(8)
15
75.047(18)
1.2647(3)
45(7)
0.15(2)
10.3(5)
0.23(5)
1.2(8)
16
76.029(11)
1.25077(1
13(4)
0.15(3)
2.5(3)
0.20(8)
0.4(5)
17
82.80(10)
1.1648(11)
8(3)
0.70(6)
6.1(5)
0.7(3)
1.4(7)
Universitas Sumatera Utara
Qualitative analysis results
Phase name
Formula
Figure of merit
Phase reg. detail
DB card number
Anatase, syn
Ti O2
0.140
ICDD (PDF-4+ 2014
01-084-1285
Zabuyelite,
Li2 ( C O3
0.760
ICDD (PDF-4+ 2014
04-010-7186
Phase
name
Formul
a
Space group
Phase reg. detail
DB card number
Anatase,
Ti O2
01-084-1285
Li2 ( C
O3 )
141 : I41/amd,choice2 : C12/c1,unique15
ICDD (PDF-4+ 2014 RDB)
Zabuyelite,
ICDD (PDF-4+ 2014 RDB)
04-010-7186
b
ll 1
Dik : Fwhm = 0,130o
B = 3,611 x 10-4 rad
2θ = 25,304 0
θ= 12, 652
cos θ = 0,9750
λ = 1,54060 x 10-10m
k = 0,94
dit : ukuran partikel (d)= ...?
penyelesaian :
ukuran kristal (d) =
𝑘𝑘 λ
B cos θ
Universitas Sumatera Utara
0,94 𝑥𝑥 1,54060 𝑥𝑥 10 −10
d = 3,611 x
10 −4 rad .0,975 0
1,448164 𝑥𝑥 10 −10
= 3,520725 x
10 −4
= 0,4113 x 10-6
= 0,4113 чm
Sampel Na2
800
Meas. data:LTO-Na/Data 1
Calc. data:LTO-Na/Data 1
Error
Residual
Intensity (counts)
600
400
200
Intensity (counts)
0
100
50
0
-50
-100
20
40
60
80
2-theta (deg)
Peak list
No
.
2theta(deg
)
d(ang.)
Height(cou
nts)
FWHM(
deg)
Int.
I(counts
deg)
Int. W(deg)
Asym.
factor
1
2
3
4
5
6
25.317(5)
36.928(16
37.802(11
38.605(14
48.043(6)
53.890(10
3.5151(7
2.4322(1
2.3780(7
2.3303(8
1.8922(2
1.6999(3
539(23)
37(6)
99(10)
33(6)
165(13)
86(9)
0.124(5)
0.13(2)
0.140(11
0.142(14
0.130(6)
0.147(11
89.2(13)
7.9(5)
17.4(6)
5.1(4)
26.8(6)
16.4(6)
0.165(9)
0.22(5)
0.18(2)
0.15(4)
0.163(16)
0.19(3)
2.1(5)
0.7(4)
1.6(5)
2.2(9)
0.89(15)
1.1(3)
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7
8
9
10
11
12
13
55.100(6)
62.113(7)
62.698(11
68.77(2)
70.281(7)
75.07(2)
82.706(14
1.66543(
1.49317(
1.4806(2
1.3640(4
1.33829(
1.2644(3
1.16588(
87(9)
26(5)
67(8)
28(5)
27(5)
42(6)
18(4)
0.126(11
0.053(17
0.132(10
0.16(2)
0.16(2)
0.17(2)
0.22(4)
15.7(7)
2.9(3)
12.2(5)
5.8(4)
5.8(4)
10.4(6)
6.3(5)
0.18(3)
0.11(3)
0.18(3)
0.21(5)
0.21(6)
0.25(5)
0.36(11)
3.1(5)
1.1(8)
1.4(7)
1.9(13)
0.6(4)
1.7(12)
1.6(11)
Qualitative analysis results
Phase
name
Formul
a
Figure of
merit
Phase reg. detail
DB card number
Anatase,
Ti O2
0.292
ICDD (PDF-4+ 2014 RDB)
01-084-1285
Phase
name
Form
ula
Space group
Phase reg. detail
DB card number
Anatase
Ti
141 :
ICDD (PDF-4+ 2014 RDB)
01-084-1285
Universitas Sumatera Utara
B
700
600
Offset Y values
500
400
300
200
100
0
24.4
24.6
24.8
25.0
25.2
25.4
25.6
25.8
26.0
A
Dik : Fwhm = 0,124o
B = 3,444 x 10-4 rad
2θ = 25,317 0
θ= 12, 6585
cos θ = 0,975690
λ = 1,54060 x 10-10m
k = 0,94
dit : ukuran partikel (d)= ...?
penyelesaian :
ukuran kristal (d) =
𝑘𝑘 λ
B cos θ
0,94 𝑥𝑥 1,54060 𝑥𝑥 10 −10
d = 3,444 x
=
10 −4 rad .0,97569 0
1,448164 𝑥𝑥 10 −10
3,36027 x 10 −4
= 0,4309 x 10-6
= 0,4309 чm
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1. PERHITUNGAN PENCAMPURAN BAHAN BAHAN
1.1 Menghitung massa bahan LTO
4LiOH.H2O + 5TiO2
Li4Ti5O12 + 3H2O
Massa atom relatif unsur :
Li = 7
Ti = 47,867
O = 15,9994
Mr LiOH.H2O
TiO2
= 41,9988
= 79,8658
Li4Ti5O12
•
= 459,3278
massa LiOH .H 2 O
1 x Mr LiOH .H 2 O
=
Massa LiOH.H2O =
=
20 gr
Mr Li 4 Ti 5 O 12
1 x Mr LiOH .H 2 O
Mr Li 4 Ti 5 O 12
1 𝑥𝑥41,9988 x 20 gr
459,3278
= 1,828707 gr
•
massa Ti O 2
1 x Mr Ti O 2
=
Massa TiO2
=
=
20 gr
Mr Li 4 Ti 5 O 12
1 x Mr Ti O 2 x 20 gr
Mr Li 4 Ti 5 O 12
1 x 79,8658 x 20 gr
459,3278
= 3,47750 gr
1.2.Menghitung massa bahan NaLiTi3O7
LiOH.H2O + 3 TiO2 + ½ Na2CO3
NaLiTi3O7 + ½ CO2 + ½ H2O + H2
Massa atom relatif unsur :
Universitas Sumatera Utara
Na = 22,989
Li = 7
Ti = 47,867
C = 12,0107
O = 15,9994
Mr LiOH.H2O = 41,9988
TiO2
= 79,8658
Na2CO3
= 105,9707
NaLiTi3O7 = 285,548
•
massa LiOH .H 2 O
1 x Mr LiOH .H 2 O
=
Massa LiOH.H2O =
=
10 gr
Mr NaLi Ti 3 O 7
1 x Mr LiOH .H 2 O x 10 gr
Mr NaLi Ti 3 O 7
1 𝑥𝑥41,9988 x 10 gr
285,548
= 1,470814 gr
•
massa Ti O 2
1 x Mr Ti O 2
=
Massa TiO2
=
=
10 gr
Mr NaLi Ti 3 O 7
1 x Mr Ti O 2 x 10 gr
Mr NaLi Ti 3 O 7
1 x 79,8658 x 10 gr
285,548
= 8,3907924 gr
•
massa Na 2 CO 3
1 x Mr Na 2 O 3
Massa Na2CO3
=
=
=
10 gr
Mr NaLi Ti 3 O 7
1 x Mr Na 2 O 3 x 10 gr
Mr NaLi Ti 3 O 7
1 x 105,9707 x 10 gr
285,548
= 1,470814 gr
Universitas Sumatera Utara
2. MENGHITUNG SPECIFIC CAPACITY TiO2
Li + TiO2 + e-
LixTiO2
Berat atom Ti = 47,867
Berat atom O = 15,999
Berat atom TiO2 = 47,867 + 2(15,999)
= 79,856 x 10-3
Specific capacity = (N x F ) / (berat atom)
Dimana : N= valensi atom
F = Konstanta Faraday (96485 colomb/mol) (26,801 Ah/mol)
Specific capacity = (1 x 26,801) / (79,865 x 10-3)
= 335,57 mAh/g
3. MENGUKUR KETEBALAN SAMPEL Li4Ti5O12 DAN NaLiTi3O12
Tebal Cu foil : 10 чm
Sampel
L (чm)
TiO2
Li4Ti5O12
NaLiTi3O12
60
90
70
L – Cu
Foil
50
80
60
Rs (Ω)
36,4
72,5
21,3
Mengukur konduktivitas
L0 = 50 x 10-6 m
L1 = 80 x 10-6 m
L2 = 70 x 10-6 m
R1 = 36,4 Ω
R1 = 72,5 Ω
R2 = 21,3 Ω
A = 5,77 mm
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Na-0 => R = ρ
L
A
50 x 10 −6 m
36,4 Ω = ρ
5,77 x 1,67 x 10 −6 m 2
50 m
36,4 Ω = ρ
5,77 x 1,67 m
ρ = 7,014 Ωm = 701,4 Ωcm
σ =
1
𝜌𝜌
1
= 701,4 Ωcm
= 0,001425 S/cm
Na-1 => R = ρ
L
A
80 x 10 −6 m
72,5 Ω = ρ
72,5 Ω = ρ
5,77 x 1,67 x 10 −6 m 2
80 m
5,77 x 1,67 m
ρ = 8,732 Ωm = 873,2 Ωcm
σ =
1
𝜌𝜌
1
= 873,2 Ωcm
= 0,00114 S/cm
Na-2 => R = ρ
L
A
21,3 Ω = ρ
21,3 Ω = ρ
70 x 10 −6 m
5,77 x 1,67 x 10 −6 m 2
70 m
5,77 x 1,67 m
ρ = 0,2932 Ωm = 293,2 Ωcm
σ =
1
𝜌𝜌
Universitas Sumatera Utara
1
= 293,2 Ωcm
= 0,00341 S/cm
4. MENGHITUNG MASSA JENIS PADA SAMPEL
Volume kosong : 43,3389 gr
Volume garis = 0,7439 cm3
Serbuk
Na0
Na1
Na2
Gr
43,8859
43,9349
43,9856
Netto
0,547
0,596
0,6467
ρSerbuk
0,7353
0,801
0,8693
Universitas Sumatera Utara
LAMPIRAN B
1.Gambar Peralatan
Beaker glass
Spatula
Beaker glass
Pipet tetes
Universitas Sumatera Utara
Penjepit
Wadah
Magnetic stirer
Ayakan
Wadah
Mortar
Universitas Sumatera Utara
Oven
Hot Plate
Oven dan Doctor Blade
Neraca digital
furnace
Pisau Doctor Blade
Universitas Sumatera Utara
Thickness gaoge
Glove box
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2. Gambar Bahan
LiOH.H2O
Na2CO3
PVDF
TiO2
DMAC
Separator
Universitas Sumatera Utara
Lithium metal
Cu foil
GAMBAR LEMBARAN
Lembaran Na0
Lembaran Na1
Lembaran Na2
Universitas Sumatera Utara
3. Gambar Alat Karaterisasi Dan Uji
Scanning Electron Microscopy (SEM)
X-Ray diffraction (XRD)
Cyclic Voltammetry dan Charge discharge
Universitas Sumatera Utara
Lampiran C
Hasil xrd TiO2, Li4Ti5O12, dan NaLiTi3O7
1. Sampel Na0
Meas. data:TiO2 china/Data 1
Calc. data:TiO2 china/Data 1
Error
Residual
Intensity (counts)
800
600
400
200
Intensity (counts)
0
100
0
-100
20
40
60
80
2-theta (deg)
Peak list
No.
2theta(deg)
d(ang.)
Height(count
s)
FWHM(deg)
Int. I(counts
deg)
Int. W(deg)
Asym. factor
1
25.284(6)
3.5196(8)
572(24)
0.134(4)
97.4(15)
0.170(10)
1.4(3)
2
36.949(7)
2.4309(4)
31(6)
0.117(17)
5.1(4)
0.16(4)
3(2)
3
37.788(8)
2.3788(5)
101(10)
0.150(9)
19.1(5)
0.19(2)
1.9(5)
4
38.555(14)
2.3332(8)
37(6)
0.120(16)
5.6(3)
0.15(3)
0.8(4)
5
48.015(6)
1.8933(2)
171(13)
0.117(6)
27.3(6)
0.159(16)
0.73(17)
6
53.847(5)
1.70118(15)
99(10)
0.122(9)
17.2(6)
0.17(2)
0.45(6)
7
55.067(7)
1.6663(2)
103(10)
0.112(9)
17.9(5)
0.17(2)
1.9(6)
8
62.13(3)
1.4929(7)
14(4)
0.19(3)
3.0(3)
0.22(9)
2.1(19)
9
62.669(11)
1.4812(2)
78(9)
0.120(9)
13.3(5)
0.17(3)
1.0(4)
10
68.745(16)
1.3644(3)
33(6)
0.142(14)
5.9(4)
0.18(4)
1.2(6)
11
70.261(11)
1.33862(18)
31(6)
0.159(15)
5.9(4)
0.19(5)
0.52(16)
12
75.067(16)
1.2644(2)
45(7)
0.167(13)
9.3(5)
0.21(4)
2.3(11)
13
76.03(3)
1.2508(4)
16(4)
0.144(19)
2.7(3)
0.17(6)
1.4(11)
Universitas Sumatera Utara
14
82.68(3)
1.1662(3)
22(5)
0.17(3)
5.3(5)
0.24(7)
1.3(10)
15
83.14(3)
1.1609(4)
10(3)
0.19(4)
2.5(4)
0.26(12)
0.7(6)
Qualitative analysis results
Phase name
Formula
Figure of merit
Phase reg. detail
DB card number
anatase, nano
Ti O2
0.144
ICDD (PDF-4+ 2014 RDB)
00-064-0863
Phase name
Formula
Space group
Phase reg. detail
DB card number
anatase, nano
Ti O2
141 : I41/amd,choice-2
ICDD (PDF-4+ 2014 RDB)
00-064-0863
Universitas Sumatera Utara
Dik : Fwhm = 0,134o
B = 3,722 x 10-4 rad
2θ = 25,284 0
θ= 12, 642
cos θ = 0,9750
λ = 1,54060 x 10-10m
k = 0,94
dit : ukuran partikel (d)= ...?
penyelesaian :
ukuran kristal (d) =
𝑘𝑘 λ
B cos θ
0,94 𝑥𝑥 1,54060 𝑥𝑥 10 −10
d = 3,722 x
=
10 −4 rad .0,975 0
1,448164 𝑥𝑥 10 −10
3,62895 x 10 −4
= 0,3990x 10-6
= 0,3990 чm
Universitas Sumatera Utara
2. Sampel Na1
Meas. data:LTO/Data 1
Calc. data:LTO/Data 1
Error
Residual
Intensity (counts)
Intensity (counts)
600
400
200
0
100
50
0
-50
-100
20
40
60
80
2-theta (deg)
Peak list
No.
2-theta(deg)
d(ang.)
Height(coun
ts)
FWHM(
deg)
Int. I(counts deg)
Int. W(deg)
Asym. factor
1
21.326(14)
4.163(3)
14(4)
0.16(4)
2.9(4)
0.21(9)
0.6(9)
2
25.304(6)
3.5169(9)
540(23)
0.130(4
90.6(14)
0.168(10)
1.5(3)
3
30.58(5)
2.921(5)
12(3)
0.25(4)
3.5(5)
0.29(12)
1.0(8)
4
31.71(4)
2.820(4)
13(4)
0.34(3)
4.6(5)
0.36(14)
0.7(3)
5
36.94(2)
2.4316(13)
36(6)
0.13(2)
6.1(4)
0.17(4)
0.9(6)
6
37.804(10)
2.3778(6)
104(10)
0.133(1
17.6(7)
0.17(2)
2.2(9)
7
38.56(3)
2.3328(16)
31(6)
0.16(2)
5.7(4)
0.19(5)
0.8(5)
8
48.048(7)
1.8920(3)
150(12)
0.134(8
26.1(7)
0.174(19)
1.4(3)
9
53.901(11)
1.6996(3)
81(9)
0.159(1
17.1(6)
0.21(3)
1.8(7)
10
55.067(9)
1.6663(2)
101(10)
0.116(8
16.0(5)
0.16(2)
1.5(5)
11
62.142(7)
1.49253(1
17(4)
0.13(2)
3.1(3)
0.18(6)
5(4)
12
62.687(10)
1.4809(2)
68(8)
0.135(1
11.7(5)
0.17(3)
0.9(3)
13
68.74(2)
1.3644(3)
26(5)
0.18(2)
6.0(4)
0.23(6)
0.7(3)
14
70.321(8)
1.33762(1
31(6)
0.150(1
6.0(3)
0.20(5)
2.6(8)
15
75.047(18)
1.2647(3)
45(7)
0.15(2)
10.3(5)
0.23(5)
1.2(8)
16
76.029(11)
1.25077(1
13(4)
0.15(3)
2.5(3)
0.20(8)
0.4(5)
17
82.80(10)
1.1648(11)
8(3)
0.70(6)
6.1(5)
0.7(3)
1.4(7)
Universitas Sumatera Utara
Qualitative analysis results
Phase name
Formula
Figure of merit
Phase reg. detail
DB card number
Anatase, syn
Ti O2
0.140
ICDD (PDF-4+ 2014
01-084-1285
Zabuyelite,
Li2 ( C O3
0.760
ICDD (PDF-4+ 2014
04-010-7186
Phase
name
Formul
a
Space group
Phase reg. detail
DB card number
Anatase,
Ti O2
01-084-1285
Li2 ( C
O3 )
141 : I41/amd,choice2 : C12/c1,unique15
ICDD (PDF-4+ 2014 RDB)
Zabuyelite,
ICDD (PDF-4+ 2014 RDB)
04-010-7186
b
ll 1
Dik : Fwhm = 0,130o
B = 3,611 x 10-4 rad
2θ = 25,304 0
θ= 12, 652
cos θ = 0,9750
λ = 1,54060 x 10-10m
k = 0,94
dit : ukuran partikel (d)= ...?
penyelesaian :
ukuran kristal (d) =
𝑘𝑘 λ
B cos θ
Universitas Sumatera Utara
0,94 𝑥𝑥 1,54060 𝑥𝑥 10 −10
d = 3,611 x
10 −4 rad .0,975 0
1,448164 𝑥𝑥 10 −10
= 3,520725 x
10 −4
= 0,4113 x 10-6
= 0,4113 чm
Sampel Na2
800
Meas. data:LTO-Na/Data 1
Calc. data:LTO-Na/Data 1
Error
Residual
Intensity (counts)
600
400
200
Intensity (counts)
0
100
50
0
-50
-100
20
40
60
80
2-theta (deg)
Peak list
No
.
2theta(deg
)
d(ang.)
Height(cou
nts)
FWHM(
deg)
Int.
I(counts
deg)
Int. W(deg)
Asym.
factor
1
2
3
4
5
6
25.317(5)
36.928(16
37.802(11
38.605(14
48.043(6)
53.890(10
3.5151(7
2.4322(1
2.3780(7
2.3303(8
1.8922(2
1.6999(3
539(23)
37(6)
99(10)
33(6)
165(13)
86(9)
0.124(5)
0.13(2)
0.140(11
0.142(14
0.130(6)
0.147(11
89.2(13)
7.9(5)
17.4(6)
5.1(4)
26.8(6)
16.4(6)
0.165(9)
0.22(5)
0.18(2)
0.15(4)
0.163(16)
0.19(3)
2.1(5)
0.7(4)
1.6(5)
2.2(9)
0.89(15)
1.1(3)
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7
8
9
10
11
12
13
55.100(6)
62.113(7)
62.698(11
68.77(2)
70.281(7)
75.07(2)
82.706(14
1.66543(
1.49317(
1.4806(2
1.3640(4
1.33829(
1.2644(3
1.16588(
87(9)
26(5)
67(8)
28(5)
27(5)
42(6)
18(4)
0.126(11
0.053(17
0.132(10
0.16(2)
0.16(2)
0.17(2)
0.22(4)
15.7(7)
2.9(3)
12.2(5)
5.8(4)
5.8(4)
10.4(6)
6.3(5)
0.18(3)
0.11(3)
0.18(3)
0.21(5)
0.21(6)
0.25(5)
0.36(11)
3.1(5)
1.1(8)
1.4(7)
1.9(13)
0.6(4)
1.7(12)
1.6(11)
Qualitative analysis results
Phase
name
Formul
a
Figure of
merit
Phase reg. detail
DB card number
Anatase,
Ti O2
0.292
ICDD (PDF-4+ 2014 RDB)
01-084-1285
Phase
name
Form
ula
Space group
Phase reg. detail
DB card number
Anatase
Ti
141 :
ICDD (PDF-4+ 2014 RDB)
01-084-1285
Universitas Sumatera Utara
B
700
600
Offset Y values
500
400
300
200
100
0
24.4
24.6
24.8
25.0
25.2
25.4
25.6
25.8
26.0
A
Dik : Fwhm = 0,124o
B = 3,444 x 10-4 rad
2θ = 25,317 0
θ= 12, 6585
cos θ = 0,975690
λ = 1,54060 x 10-10m
k = 0,94
dit : ukuran partikel (d)= ...?
penyelesaian :
ukuran kristal (d) =
𝑘𝑘 λ
B cos θ
0,94 𝑥𝑥 1,54060 𝑥𝑥 10 −10
d = 3,444 x
=
10 −4 rad .0,97569 0
1,448164 𝑥𝑥 10 −10
3,36027 x 10 −4
= 0,4309 x 10-6
= 0,4309 чm
Universitas Sumatera Utara