IDAWATI SUPU
SEKOLAH PASCASARJANA INSTITUT PERTANIAN BOGOR
BOGOR 2014
33 serta kajian lebih jauh tentang fikosianin dan interaksinya dengan TiO2. Selain itu, proses pengadukan TiO2 dapat dilakukan pada autoclave reaktor hydrothermal sehingga suhu lebih terkontrol (vakum).
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Lampiran 1 Media modifikasi teknis (MT) untuk pertumbuhan S. platensis
Bahan Jumlah (g/L) (Hastuti 2011) MgSO4 0,02 CaCl2 0,004 Na2EDTA 0,008 K2SO4 0,04 FeCl3 0,001 NaHCO3 2 (NH4)2 CO 0,13 (NH4)2 SO4 0,06 Na2HPO4 0,04 Vit B12 1 mL
37 Lampiran 2 Data JCPDS (21-1272) kristal TiO2 fase anantase
38
39 Lampiran 4 Data XRD pada suhu kalsinasi 400oC
2θ θ θ
(rad) FWHM
FWHM
(rad) cos θ σ (nm) σ rata
-rata (nm) h k l d hkl (A) a (A) c (A)
25,32 12,66 0,22 0,6044 0,0105 0,9757 13,3218 13,7549 1 0 1 2,4969 3,6577 10,0012 37,76 18,88 0,33 0,6593 0,0115 0,9462 12,5932 0 0 4 1,3127 48,12 24,06 0,42 0,6489 0,0113 0,9131 13,2585 2 0 0 1,0728 53,94 26,97 0,47 0,6600 0,0115 0,8912 13,3555 1 0 5 1,9849 62,70 31,35 0,55 0,7400 0,0129 0,8540 12,4310 2 0 4 1,9146 68,74 34,37 0,60 0,6200 0,0108 0,8254 15,3511 1 1 6 1,8193 75,02 37,51 0,65 0,6200 0,0108 0,7932 15,9735 2 1 5 1,7505
α ϒ δ sin^2θ α^2 ϒ^2 δ^2 αϒ αδ ϒδ αsin^2θ ϒsin^2θ δsin^2θ
0 0 1,8290 0,0347 0 0 3,3454 0 0,0000 0,0000 0,0000 0,0000 0,0634 0 0 3,7498 0,0037 0 0 14,0609 0 0,0000 0,0000 0,0000 0,0000 0,0139 1 1 5,5435 0,7045 1 1 30,7300 1 5,5435 5,5435 0,7045 0,7045 3,9055 0 0 6,5351 0,2581 0 0 42,7078 0 0,0000 0,0000 0,0000 0,0000 1,6868 1 1 7,8964 0,0173 1 1 62,3532 1 7,8964 7,8964 0,0173 0,0173 0,1365 2 4 8,6852 0,1342 4 16 75,4328 8 17,3704 34,7408 0,2684 0,5367 1,1654 1 1 9,3319 0,1364 1 1 87,0838 1 9,3319 9,3319 0,1364 0,1364 1,2725 ∑ 7 43,571 1,28884 7 19 315,714 11 40,1422 57,5126 1,1265 1,3949 8,2440
40
Lampiran 5 Data XRD pada suhu kalsinasi 600oC
2θ θ (rad) θ FWHM FWHM (rad) cos θ σ (nm) σ rata(nm) -rata h k l d hkl (A) a (A) c (A)
25,36 12,68 0,2213 0,4823 0,0084 0,9756 16,8833 20,7964 1 0 1 5,5168 3,0895 10,5706 37,78 18,89 0,3297 0,5170 0,0090 0,9461 16,2407 0 0 4 1,3182 48,08 24,04 0,4196 0,4962 0,0087 0,9133 17,5307 2 0 0 1,4171 53,88 26,94 0,4702 0,5518 0,0096 0,8915 16,1495 1 0 5 1,9884 54,94 27,47 0,4794 0,5518 0,0096 0,8873 16,2264 2 1 1 1,0498 62,62 31,31 0,5465 0,6495 0,0113 0,8544 14,3162 2 0 4 1,9147 68,72 34,36 0,5997 0,4927 0,0086 0,8255 19,5321 1 1 6 1,8182 69,76 34,88 0,6088 0,1800 0,0031 0,8204 53,7997 2 2 0 1,8182 74,98 37,49 0,6543 0,6072 0,0106 0,7935 16,4891 2 1 5 1,7515
α ϒ δ sin^2θ α^2 ϒ^2 δ^2 αϒ αδ ϒδ αsin^2θ ϒsin^2θ δsin^2θ
1 1 1,8344 0,0482 1 1 3,3652 1 1,8344 1,8344 0,0482 0,0482 0,0884 0 16 3,7532 0,1048 0 256 14,0863 0 0,0000 60,0507 0,0000 1,6770 0,3934 4 0 5,5365 0,1660 16 0 30,6531 0 22,1461 0,0000 0,6638 0,0000 0,9188 1 25 6,5252 0,2053 1 625 42,5776 25 6,5252 163,1288 0,2053 5,1315 1,3394 7 1 6,7003 0,2128 49 1 44,8934 7 46,9018 6,7003 1,4895 0,2128 1,4257 4 16 7,8850 0,2701 16 256 62,1734 64 31,5401 126,1602 1,0802 4,3209 2,1294 3 36 8,6828 0,3185 9 1296 75,3918 108 26,0485 312,5825 0,9556 11,4673 2,7658 12 0 8,8032 0,3270 144 0 77,4957 0 105,6380 0,0000 3,9243 0,0000 2,8788 7 25 9,3284 0,3704 49 625 87,0187 175 65,2987 233,2095 2,5930 9,2605 3,4554 ∑ 120 59,0490 2,02303 285 3060 437,6553 380 305,9327 903,6665 10,9598 32,1183 15,3951
41 Lampiran 6 Data XRD pada suhu kalsinasi 800oC
2θ θ (rad) θ FWHM FWHM
(rad) cos θ σ (nm) σ rata(nm) -rata h k l d hkl (A) a (A) c (A)
25,4 12,7 0,2217 0,2907 0,0051 0,9755 28,0133 25,2476 1 0 1 1,3975 3,7812 10,2243 36,9 18,45 0,3220 0,2931 0,0051 0,9486 28,5728 1 0 3 1,3060 37,86 18,93 0,3304 0,3025 0,0053 0,9459 27,7635 0 0 4 1,4127 37,96 18,98 0,3313 0,3218 0,0056 0,9456 26,1062 1 1 2 1,9800 48,08 24,04 0,4196 0,3169 0,0055 0,9133 27,4495 2 0 0 1,0463 53,88 26,94 0,4702 0,4177 0,0073 0,8915 21,3342 1 0 5 1,9104 55,04 27,52 0,4803 0,3482 0,0061 0,8868 25,7261 2 1 1 1,8156 62,68 31,34 0,5470 0,3451 0,0060 0,8541 26,9526 2 0 4 1,8156 68,66 34,33 0,5992 0,4482 0,0078 0,8258 21,4637 1 1 6 1,7468 70,31 35,16 0,6136 0,4192 0,0073 0,8176 23,1788 2 2 0 1,9885 74,98 37,49 0,6543 0,4731 0,0083 0,7935 21,1629 2 1 5 1,0463
α ϒ δ sin^2θ α^2 ϒ^2 δ^2 αϒ αδ ϒδ αsin^2θ ϒsin^2θ δsin^2θ
1 1 1,8399 0,0483 1 1 3,3851 1 1,8399 1,8399 0,0483 0,0483 0,0889 1 9 3,6050 0,1002 1 81 12,9963 9 3,6050 32,4454 0,1002 0,9014 0,3611 0 16 3,7667 0,1052 0 256 14,1880 0 0,0000 60,2671 0,0000 1,6839 0,3964 3 4 3,7836 0,1058 9 16 14,3158 12 11,3509 15,1345 0,3173 0,4231 0,4002 4 0 5,5365 0,1660 16 0 30,6531 0 22,1461 0,0000 0,6638 0,0000 0,9188 1 25 6,5252 0,2053 1 625 42,5776 25 6,5252 163,1288 0,2053 5,1315 1,3394 7 1 6,7167 0,2135 49 1 45,1135 7 47,0166 6,7167 1,4945 0,2135 1,4340 4 16 7,8936 0,2705 16 256 62,3083 64 31,5742 126,2970 1,0821 4,3283 2,1354 3 36 8,6758 0,3180 9 1296 75,2687 108 26,0273 312,3272 0,9541 11,4498 2,7593 12 0 8,8648 0,3315 144 0 78,5842 0 106,3773 0,0000 3,9784 0,0000 2,9390 7 25 9,3284 0,3704 49 625 87,0187 175 65,2987 233,2095 2,5930 9,2605 3,4554 ∑ 133 66,5360 2,2348 295 3157 466,4094 401 321,7611 951,3660 11,4370 33,4404 16,2279
42
Lampiran 7 Data XRD pada suhu kalsinasi 1000 0C
2θ θ θ (rad) FWHM FWHM
(rad) cos θ σ (nm) σ rata(nm) -rata h k l d hkl
(A) a (A) c (A)
27,5 13,75 0,2400 0,1698 0,0030 0,9713 48,1662 48,8846 1 1 0 1,8946 4,9935 2,2243 36,14 18,07 0,3154 0,1877 0,0033 0,9507 44,5199 1 0 1 1,3074 39,2 19,6 0,3421 0,2044 0,0036 0,9421 41,2566 2 0 0 1,4139 41,28 20,64 0,3602 0,2120 0,0037 0,9358 40,0430 1 1 1 0,9810 44,06 22,03 0,3845 0,2073 0,0036 0,9270 41,3408 2 1 0 1,0472 54,38 27,19 0,4746 0,2389 0,0042 0,8895 37,3845 2 1 1 0,9112 56,66 28,33 0,4945 0,2343 0,0041 0,8802 38,5198 2 2 0 0,8163 62,94 31,47 0,5493 0,1739 0,0030 0,8529 53,5609 0 0 2 0,8163 64,06 32,03 0,5590 0,2756 0,0048 0,8478 32,0022 3 1 0 1,2546 69,02 34,51 0,6023 0,1702 0,0030 0,8240 56,6436 3 0 1 0,7475 69,76 34,88 0,6088 0,1614 0,0028 0,8204 59,9996 1 1 2 1,2460 75,4 37,7 0,6580 0,1316 0,0023 0,7912 76,2952 2 0 2 1,3007
α ϒ δ sin^2θ α^2 ϒ^2 δ^2 αϒ αδ ϒδ αsin^2θ ϒsin^2θ δsin^2θ
3 0 2,1321 0,0565 9 0 4,5459 0 6,3964 0,0000 0,1695 0,0000 0,1205 1 1 3,4782 0,0962 1 1 12,0977 1 3,4782 3,4782 0,0962 0,0962 0,3346 4 0 3,9946 0,1125 16 0 15,9569 0 15,9784 0,0000 0,4501 0,0000 0,4495 3 1 4,3526 0,1243 9 1 18,9448 3 13,0577 4,3526 0,3728 0,1243 0,5408 7 0 4,8360 0,1407 49 0 23,3866 0 33,8518 0,0000 0,9849 0,0000 0,6804 7 1 6,6080 0,2088 49 1 43,6660 7 46,2562 6,6080 1,4616 0,2088 1,3797 12 0 6,9793 0,2252 144 0 48,7111 0 83,7520 0,0000 2,7024 0,0000 1,5717 0 4 7,9304 0,2725 0 16 62,8920 0 0,0000 31,7218 0,0000 1,0902 2,1614 13 0 8,0872 0,2813 169 0 65,4034 0 105,1341 0,0000 3,6572 0,0000 2,2751 9 1 8,7181 0,3210 81 1 76,0046 9 78,4625 8,7181 2,8888 0,3210 2,7983 3 4 8,8032 0,3270 9 16 77,4957 12 26,4095 35,2127 0,9811 1,3081 2,8788 4 4 9,3646 0,3740 16 16 87,6959 16 37,4584 37,4584 1,4959 1,4959 3,5020 ∑ 16 75,2843 2,5400 552 52 536,8005 48 450,2351 127,5497 15,2603 4,6443 18,6929
43 Lampiran 8 Performa sel kalsinasi 400oC
Voc Isc Isc P FF η (%)
(mV) (µA) (mA) (mWatt)
5,2 0,26 0,00026 0,001352 0,544 0,06 6,3 0,26 0,00026 0,001638 7,8 0,26 0,00026 0,002028 9,7 0,26 0,00026 0,002522 10,9 0,26 0,00026 0,002834 11,8 0,26 0,00026 0,003068 12,7 0,26 0,00026 0,003302 13,9 0,26 0,00026 0,003614 20,815 0,2559 0,000256 0,005327 30,762 0,2374 0,000237 0,007303 33,849 0,2232 0,000223 0,007555 40,709 0,1394 0,000139 0,005675 50,999 0,0217 0,0000217 0,001107 53,4 0,0179 0,0000179 0,000956
44
Lampiran 9 Performa sel kalsinasi 600oC
Voc Isc Isc P FF η (%)
(mV) (µA) (mA) (mWatt)
6 0,61 0,00061 0,003660 0,352 0,29 11,2 0,66 0,00066 0,007392 20,7 0,65 0,00065 0,013455 36,9 0,63 0,00063 0,023247 49,7 0,59 0,00059 0,029323 55,4 0,58 0,00058 0,032132 67 0,51 0,00051 0,034170 78,9 0,45 0,00045 0,035505 90 0,37 0,00037 0,033300 98,8 0,33 0,00033 0,032604 107,9 0,27 0,00027 0,029133 120,1 0,22 0,00022 0,026422 130,7 0,15 0,00015 0,019605 134,4 0,13 0,00013 0,017472
45 Lampiran 10 Performa sel kalsinasi 800oC
Voc Isc Isc P FF η (%)
(mV) (µA) (mA) (mWatt)
19,8 0,89 0,00089 0,017622 0,640 1,04 39,2 0,89 0,00089 0,034888 68,2 0,89 0,00089 0,060698 121 0,84 0,00084 0,101640 130 0,83 0,00083 0,107900 148,8 0,82 0,00082 0,122016 152,5 0,81 0,00081 0,123525 154,1 0,81 0,00081 0,124821 157 0,77 0,00077 0,120890 158,2 0,76 0,00076 0,120232 167,4 0,72 0,00072 0,120528 176,9 0,67 0,00067 0,118523 208,9 0,46 0,00046 0,096094 229,9 0,38 0,00038 0,087362 239,9 0,34 0,00034 0,081566 249,7 0,27 0,00027 0,067419 260,1 0,23 0,00023 0,059823 280 0,16 0,00016 0,044800 296 0,12 0,00012 0,035520 318 0,02 0,00002 0,006360
RINGKASAN
IDAWATI SUPU. Penggunaan fikosianin dari mikroalga Spirulina platensis
sebagai light harvesting pada sel suryananopartikel TiO2 anatase. Dibimbing oleh AKHIRUDDIN MADDU dan IRIANI SETYANINGSIH.
Pembuatan dye sensitized solar cell (DSSC) dilakukan menggunakan film hibrid nanopartikel tatanium oksida (TiO2)/fikosianin. Sintesis TiO2 dengan metode sol gel dari titanium klorida (TiCl4) sebagai prekursor melalui tahap hidrolisis menggunakan asam sulfat (H2SO4). Selanjutnya dipanaskan pada tanur (furnace) selama 2,5 jam dengan suhu berbeda (400oC, 600oC, 800oC, dan 1000oC). Pola XRD menunjukkan bahwa fase yang muncul pada suhu pemanasan 400oC sampai 800oC hanya anatase. Ketika suhu dinaikkan sampai 1000oC, terjadi transformasi fase dari anatase menjadi rutil. Berdasarkan hasil XRD diperoleh ukuran kristal dan partikel masing-masing 13,75 nm, 20,79 nm, 25,25 nm, 48,88 nm dan SEM diperoleh ukuran partikel 43,06 nm, 44,91 nm dan 64,99 nm dan 80,40 nm. Ukuran kristal dan ukuran partikel meningkat seiring dengan peningkatan suhu. Pengukuran sifat optik film TiO2 dan hibrid TiO2/fikosianin menggunakan spektrofotometer UV-Vis. Penambahan fikosianin mampu menambah lebar serapan dari daerah ultraviolet (UV) sampai daerah tampak (visible).
Energi celah dapat ditentukan dari hasil karakteristik film optik, yaitu berdasarkan perpotongan kurva bagian linear dengan sumbu energi (hv). Pada penelitian ini, hanay dibatasi pada fase anatase saja. Hal ini disebabkan karena energi gap anatase yang lebih lebar jika dibandingkan fase rutil. Dengan demikian, sangat berarti dalam aplikasi sel surya seperti dye sensitized solar cell (DSSC). Hasil perhitugan koefisien absorpsi rata-rata dari masing-masing suhu kalsinasi 400oC, 600oC, 800oC berturut-turut adalah 8,1600x102, 1,7535x103, dan 4,0154x102 lebih kecil dari 104 sehingga termasuk transisi langsung. Nilai energi celah pada kalsinasi 400oC, 600oC, 800oC masing-masing 3,79 eV, 3,58 eV dan 3,35 eV. Peningkatan suhu kalsinasi menyebabkan penurunan energi celah semikonduktor TiO2.
Kultivasi Spirulina platensis dilakukan dengan media MT (media teknis modifikasi Hastuti). Kepadatan sel optimum ( fase stasioner) pada hari ke-8 dengan nilai OD > 0,5. Pada keadaan tersebut, kultur dapat dipanen. Inokulum
S.platensis yang dikultur dari 80 literdihasilkan berat kering biomassa 10,46 gram dan bobot fikosianin dalam bentuk bubuk kering 5,50 gram. Daerah serapan tertinggi fikosianin berada pada panjang gelombang 619,36 nm (daerah visible) dengan energi relaksasi 2,945 eV. Spektrum emisi tertinggi pada panjang gelombang 708,55 nm dengan energi relaksasi 2,793 eV. Nilai pergeseran Stokes berdasarkan perbedaan transisi absorpsi dan emisi fikosianin adalah 0,152 eV.
Integrasi antara protein pemanen cahaya dengan permukaan semikonduktor TiO2 memiliki peranan penting dalam meningkatkan performa sebagai material sel surya. Gugus karboksilat (-COOH) dapat menjadikan dye lebih efisien karena melekat pada permukaan ampoter oksida TiO2. Pigmen fikosianin memiliki gugus karboksilat sehingga bereaksi dengan permukaan oksida dengan membentuk ester. Gugus karboksilat tersebut dapat menaikkan pasangan elektronik dye dari tingkat
eksitasi (molekul orbital yang memiliki orbital p anti bonding) menuju tingkat akseptor semikonduktor (pita konduksi TiO2).
Sampel yang telah dibuat berdasarkan variasi suhu masing-masing dibentuk sel surya. Selanjutnya sel surya dirangkai untuk pengujian karakteristik arus-tegangan (I-V) di bawah sinar matahari langsung sebagai sumber cahaya dengan intensitas ± 120 Watt/m2. Kurva terdiri atas beberapa parameter seperti arus hubungan singkat Isc (short circuit) yaitu arus ketika potensial sama dengan nol, tegangan rangkaian terbuka Voc (open circuit voltage) yaitu tegangan ketika beban luar diberikan sangat besar, Vmax yaitu tegangan yang memberikan nilai daya maksimum, dan Imax yaitu arus yang memberikan nilai daya maksimum. Faktor pengisi atau fill factor (FF) adalah perbandingan antara perkalian arus maksimum dan tegangan maksimum dengan perkalian Voc dan Isc. Efisiensi merupakan perbandingan antara daya yang dihasilkan sel surya dengan daya cahaya yang mengenai sel surya tersebut.
Kemampuan sel mengkonversi energi matahari menjadi energi listrik dengan efisiensi tertinggi dihasilkan dari sel dengan kalsinasi 800oC yaitu 1,04%. Pada suhu 400oC, efisiensi yang dihasilkan yaitu 0,06 lebih kecil jika dibandingkan sel pada suhu 600oC sebesar 0,29%. Dari ketiga jenis sel diperoleh nilai tegangan open-circuit (Voc) dan rapat arus (Isc) semakin meningkat seiring dengan peningkatan suhu kalsinasi TiO2. Semakin tinggi suhu kalsinasi TiO2 maka efisiensi yang dihasilkan makin meningkat.
SUMMARY
IDAWATI SUPU. Application of phycocyanin from microalgae Spirulina platensis as light harvesting in anatase TiO2 nanoparticle solar cell. Supervised by AKHIRUDDIN MADDU and IRIANI SETYANINGSIH.
The dye sensitized solar cell (DSSC) has been assemblied used hybrid titanium oxide (TiO2) film/phycocyanin. The TiO2 film was synthesizedby sol gel method with titanium chlorida (TiCl4) as precursor by hydrolysis used sulfuric acid (H2SO4). Furthermore, it calcinated for 2,5 hours in variation of annealing temperature (400oC, 600oC, 800oC, dan 1000oC). In XRD patterns exhibited which annealing temperature at 400oC to 800oC were anatase phase all. When annealed at temperature 1000oC, it caused phase transformation from anatase to rutile. The crystals size according to XRD patterns were 13,75 nm, 20,79 nm, 25,25 nm, 48,88 nm and particle size from SEM images were 43,06 nm, 44,91 nm dan 64,99 nm, 80,40 nm, respectively. The crystals and particle size increased with annealing temperature. The film thickness influenced material absorption. The optical measurement of TiO2 film and TiO2/phycocyanin hybrid film used UV-Vis spectrophotometer. Additional phycocyanin caused peak width of absorbed region from ultraviolet to visible region.
The band gap energy of TiO2 can be calculated using the cut off wavelength obtained from the absorbance spectrum of a nanoparticles TiO2 films. Based on intersection between linear and energy (hv) axis. In this study just limited for anatase phase. It was caused anatase band gap is wider than rutile phase. That’s meaningful for solar cell application such as dye sensitized solar cell (DSSC). The absorption coefficient average at difference annealing temperature such as at 400oC, 600oC, 800oC were 8,1600x102, 1,7535x103 and 4,0154x102, where α < 104 include to direct transition. Band gap energy 400oC, 600oC, 800oC were 3,79 eV, 3,59 eV, and 3,35 eV, respectively. Based on this result, exhibition that band gap energy of TiO2 semiconductor film decreased with increasing annealing temperature.
Spirulina platensis was cultivated in technical modification (Hastuti) with aeration under light intensity about 3000 lux. The cell density (stationer phase) for eighth day which OD value was more than 0,5. It means, the culture can be harvested. In 80 liters Spirulina platensis culture have been produced biomass dry about 10,46 gram and extracted phycocyanin in dry powders was 5,50 gram. The phycocyanin absorption spectrum at the wavelength of 619,36 nm (visible region) which had relaxation energy was 2,945 eV. The emission peak at the wavelength of 708,55 nm with relaxation energy about 2,793 eV. The Stokes shift based on difference energy absorption and emission calculated about 0,152 eV. Both of this showed phycocyanin can absorbed and radiated the sun light which received. This choice characteristic pigment was a good one related to sensitizer in solar cell application.
Integration between light harvesting protein and TiO2 semiconductor surface had important role in improving of output as solar cell materials. The presence of carboxylate group (-COOH) made pigment be more efficient was due to anchored to the surface of TiO2 ampoter. The phycocyanin pigment had carboxylate group
which reacted with TiO2 surface formed ester. The carboxylate group increased of dye electronics couple from excited state (p anti bonding orbital) to semiconductor acceptor state (TiO2 conduction band).
The samples which made based on annealing temperature variation formed be solar cell respectively. Furthermore, cells be assembled for current-voltage (I-V) measurement under direct sun light with intensity about 120 Watt/m2. The measurement result consists of Isc (short circuit) if voltage was zero, Voc (open circuit voltage) where external load was highest, Vmax when voltage provided maximum power and Imax when current produced maximum power. The fill factor (FF) was ratio between Vmax Imax and Voc Isc. The efficiency be calculated by comparison between power of solar cell result and light power which attracted.
The cell potentiality converted sunlight into electrical energy with highest efficiency resulted for cell at 800oC calcinated temperature was 1,04%. The annealing temperature at 400oC lesser than cell calcinated at 600oC was 0,29%. From the result, Voc and Isc increased with increasing of TiO2 annealing temperature. Moreover, increasing of annealing temperature increased to the efficiency result.