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Ratnawati
Abstrak :
[ABSTRAK
Sintesis TiO2 bermorfologi nanotube array bentuk film (TNTAs) telah dilakukan dengan proses anodisasi logam Ti dalam larutan elektrolit gliserol yang mengandung NH4F, dilanjutkan dengan annealing untuk membuat fasa kristal dari TNTAs. Optimasi berbagai parameter meliputi variasi kadar air dalam larutan elektrolit, perlakuan annealing, penambahan NaBF4, metode dan lama pengadukan serta variasi loading dan metode dalam penambahan dopan logam Pt. Hasil SEM/FESEM menunjukkan bahwa TNTAs berhasil disintesis dengan tube yang rapi, tegak lurus dan mempunyai kisaran diameter dalam antara 49-205 nm, tebal dinding 11-33 nm serta panjang 530-2577 nm. Annealing dengan H2/Ar merupakan cara yang efisien untuk memasukkan dopan C, N dan B dalam matrik TNTAs secara insitu saat anodisasi, sehingga diperoleh penurunan energi band gap sampai pada kisaran 2,20?3,10 eV. Kebanyakan TNTAs berfasa anatase dengan ukuran kristal dari 18?33 nm. TNTAs yang disintesis pada kadar air 25% volume dan annealing dengan 20% H2/Ar merupakan fotokatalis optimal yang menghasilkan kerapatan arus tertinggi. Uji TNTAs untuk memproduksi hidrogen menggunakan gliserol sebagai sacrificial agent. Penambahan 5 mM NaBF4 selama anodisasi menghasilan TNTAs termodifikasi yang mampu menghambat laju rekombinasi elektron-hole sehingga dapat meningkatkan produksi hidrogen sebesar 32 %. Penambahan dopan Pt sebagai electron trapper secara fotodeposisi pada TNTAs hasil anodisasi ultrasonik mampu menghasilkan hidrogen dari larutan gliserol sebesar lima kali lebih tinggi dibandingkan tanpa penambahan Pt.;
ABSTRACT
Synthesis of TiO2 nanotube array (TNTAs) has been performed by anodization process of Ti metal in the glycerol electrolyte solution containing NH4F followed by annealing to induce crystallization. Optimization some parameters was done including the variation of water content in the electrolyte solution, annealing atmosphere, addition of NaBF4, mode of mixing, as well as the variation of loading and the methods of Pt addition on the TNTAs. SEM/FESEM analysis showed that well ordered and vertically oriented of TNTAs with inner diameters of 49-205 nm, wall thicknesses from 11 to 33 nm and lengths from 530 to 2577 nm were synthesized. Annealing with H2/Ar is found to be an efficient method for introducing dopant C, N and B into the lattice of TNTAs via insitu anodization and, therefore, the reducing band gap in the range of 2,20?3,10 eV can be obtained. Most of TNTAs have anatase phase with the crystalline size from 18 to 33 nm. Water content of 25 v% and annealing under H2/Ar of as-synt TNTAs showed optimal condition in producing the highest photocurrent density. The photocatalytic hydrogen production test was performed with glycerol as a sacrificial agent. The addition of 5 mM NaBF4 during anodization resulted modified TNTAs that can reduce recombination of electron-hole and showed up 32 % improvement in hydrogen production. The photodeposition of Pt on the TNTAs that obtained from ultrasonic anodization can enhance hydrogen production five times higher compare to the one with unplatinized TNTAs.;Synthesis of TiO2 nanotube array (TNTAs) has been performed by anodization process of Ti metal in the glycerol electrolyte solution containing NH4F followed by annealing to induce crystallization. Optimization some parameters was done including the variation of water content in the electrolyte solution, annealing atmosphere, addition of NaBF4, mode of mixing, as well as the variation of loading and the methods of Pt addition on the TNTAs. SEM/FESEM analysis showed that well ordered and vertically oriented of TNTAs with inner diameters of 49-205 nm, wall thicknesses from 11 to 33 nm and lengths from 530 to 2577 nm were synthesized. Annealing with H2/Ar is found to be an efficient method for introducing dopant C, N and B into the lattice of TNTAs via insitu anodization and, therefore, the reducing band gap in the range of 2,20?3,10 eV can be obtained. Most of TNTAs have anatase phase with the crystalline size from 18 to 33 nm. Water content of 25 v% and annealing under H2/Ar of as-synt TNTAs showed optimal condition in producing the highest photocurrent density. The photocatalytic hydrogen production test was performed with glycerol as a sacrificial agent. The addition of 5 mM NaBF4 during anodization resulted modified TNTAs that can reduce recombination of electron-hole and showed up 32 % improvement in hydrogen production. The photodeposition of Pt on the TNTAs that obtained from ultrasonic anodization can enhance hydrogen production five times higher compare to the one with unplatinized TNTAs., Synthesis of TiO2 nanotube array (TNTAs) has been performed by anodization process of Ti metal in the glycerol electrolyte solution containing NH4F followed by annealing to induce crystallization. Optimization some parameters was done including the variation of water content in the electrolyte solution, annealing atmosphere, addition of NaBF4, mode of mixing, as well as the variation of loading and the methods of Pt addition on the TNTAs. SEM/FESEM analysis showed that well ordered and vertically oriented of TNTAs with inner diameters of 49-205 nm, wall thicknesses from 11 to 33 nm and lengths from 530 to 2577 nm were synthesized. Annealing with H2/Ar is found to be an efficient method for introducing dopant C, N and B into the lattice of TNTAs via insitu anodization and, therefore, the reducing band gap in the range of 2,20–3,10 eV can be obtained. Most of TNTAs have anatase phase with the crystalline size from 18 to 33 nm. Water content of 25 v% and annealing under H2/Ar of as-synt TNTAs showed optimal condition in producing the highest photocurrent density. The photocatalytic hydrogen production test was performed with glycerol as a sacrificial agent. The addition of 5 mM NaBF4 during anodization resulted modified TNTAs that can reduce recombination of electron-hole and showed up 32 % improvement in hydrogen production. The photodeposition of Pt on the TNTAs that obtained from ultrasonic anodization can enhance hydrogen production five times higher compare to the one with unplatinized TNTAs.]
2015
D2057
UI - Disertasi Membership  Universitas Indonesia Library
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Desi Heltina
Abstrak :
Limbah fenol merupakan salah satu bahan buangan berbahaya yang dapat menimbulkan permasalahan bagi lingkungan. Upaya yang dilakukan untuk mengatasi masalah tersebut adalah dengan mengeliminasi fenol. Proses fotokatalisis dapat digunakan untuk mendegradasi senyawa fenol. TiO2 nanotube TiNT merupakan salah satu diantara beberapa material fotokatalis. Untuk meningkatkan kinerja fotokatalis dalam mendegradasi fenol diperlukan kombinasi dengan proses adsorpsi. Carbon nanotube CNT memiliki kemampuan adsorpsi yang baik dan dapat bertindak sebagai penangkap elektron elektron trapping sehingga dapat dikombinasi dengan TiNT. Kombinasi TiNT dan CNT dapat meningkatkan kinerja fotokatalis dalam mendegradasi fenol. Rekayasa komposit TiNT-CNT bertujuan untuk mendapatkan material TiNT dan komposit TiNT-CNT. Kinerja komposit TiNT-CNT diuji efektivitasnya dalam mendegradasi fenol. Penelitian ini diinvestigasi terhadap sintesis, karakterisasi dan aktivitas fotokatalis TiNT dan komposit TiNT-CNT. TiNT disintesis dari TiO2 P25 nanopartikel yang ditambahkan NaOH dengan metode hidrotermal pada suhu 130oC, kecepatan 600 rpm selama 6 jam. Variasi yang dilakukan adalah lama waktu pencucian dengan HCl, waktu hidrotermal dan suhu kalsinasi. Hal ini bertujuan untuk mendapatkan TiNT yang memenuhi kriteria nanotube dan mempunyai kinerja fotokatalis dalam mendegradasi fenol. Treatment CNT menggunakan asam HNO3 dan surfaktan cocoPAS bertujuan untuk menghasilkan gugus fungsional CNT sehingga gugus fungsional tersebut diharapkan dapat berikatan dengan gugus fungsional TiNT. Sedangkan penambahan surfaktan bertujuan menghasilkan dispersi CNT dan TiNT. Komposit terjadi karena adanya interaksi elektrostatik antara TiNT dan CNT. Sintesis komposit TiNT-CNT dengan CNT yang sudah dimodifikasi dengan perlakuan asam dan surfaktan cocoPAS menggunakan metode pengadukan selama 3 jam. Kinerja komposit TiNT-CNT diuji efektivitasnya dalam mendegradasi fenol. Hasil karakterisasi diperoleh bahwa TiNT mempunyai morfologi nanotube pada waktu hidrotermal selama 6 jam dan lama waktu pencucian dengan HCl adalah 1 jam. Kinerja fotokatalis TiNT yang paling maksimum dalam mengeliminasi fenol adalah TiNT pada kalsinasi 700 C dengan persen degradasi sebesar 54. Diperoleh TiNT yang memiliki struktur kristal anatase dengan ukuran 27 nm, luas permukaan spesifik 29,7 m2/g. Proses perlakuan asam pada CNT berhasil meningkatkan jumlah oksigen dalam carbon yang mengarah pada terbentuknya gugus fungsional karboksilat pada permukaan CNT. Sedangkan proses penambahan surfaktan mampu mendispersi senyawa komposit TiNT-CNT. Kristalinitas dan ukuran kristal katalis merupakan parameter yang paling mempengaruhi aktivitas fotokatalisis disamping luas permukaan dan morfologi. Pada komposit TiNT-CNT morfologi yang diperoleh berbentuk acak. Kinerja paling tinggi dalam mendegradasi fenol adalah fotokatalis komposit TiNT-CNT dengan CNT yang ditreatment asam HNO3. Loading maksimum CNT dalam komposit TiNT-CNT adalah sebesar 2 yang mempunyai kinerja untuk eliminasi fenol sebesar 62. Dari hasil yang diperoleh dapat dinyatakan bahwa rekayasa komposit Titania nanotube TiNT dan Carbon nanotube CNT mempunyai potensi yang menjanjikan sebagai alternatif dalam mengolah limbah fenol.
Phenol waste is one of the hazardous waste materials that can cause problems for the environment. Efforts are made to overcome the problem is to eliminate phenol. The photocatalytic process can be used to degrade the phenol compounds. TiO2 nanotubes TiNT is one of several photocatalyst materials. To improve the performance of photocatalyst in degrading phenol is required combined with the adsorption process. Carbon nanotubes CNTs have excellent adsorption capability and can act as electron trapping electron trapping so that it can be combined with TiNT. The combination of TiNT and CNT can improve the performance of photocatalyst in degrading phenol. TiNT CNT composite design aims to obtain TiNT and TiNT CNT composite materials. The performance of TiNT CNT composites tested its effectiveness in degrading phenol. This study investigated the synthesis, characterization and activity of TiNT photocatalysts and TiNT CNT composites. The TiNT was synthesized from TiO2 P25 nanoparticles added NaOH by hydrothermal method at 130oC, 600 rpm for 6 hours. The variations performed were the length of washing time with HCl, hydrothermal time and calcination temperature. It aims to obtain TiNT that meets the nanotube criteria and has a photocatalytic performance in degrading phenol. Treatment of CNTs using acid HNO3 and surfactant cocoPAS aims to produce CNT functional groups so that the functional groups are expected to bind to the TiNT functional group. While the addition of surfactant aims to produce CNT and TiNT dispersions. Composites occur because of the electrostatic interaction between TiNT and CNT. The synthesis of TiNT CNT composites with modified CNTs with acid and surfactant treatments cocoPAS using a stirring method for 3 hours. The performance of TiNT CNT composites tested its effectiveness in degrading phenol. The characterization results show that TiNT has nanotube morphology at the hydrothermal time for 6 hours and the washing time with HCl is 1 hour. The maximum TiNT photocatalyst performance in eliminating phenol is TiNT at calcination of 700 C with 54 degradation percentage. TiNT has an anatase crystalline structure of 27 nm in size, a specific surface area of 29.7 m2 g. The acid treatment process of CNTs has successfully increased the amount of oxygen in the carbon that leads to the formation of carboxylic functional groups on the CNT surface. While the process of addition of a surfactant is able to disperse the compound TiNT CNT. The crystallinity and crystal size of the catalyst is the parameters that most influence the activity of photocatalysis in addition to surface area and morphology.In the morphologically obtained TiNT CNT composite obtained randomly. The highest performance in degrading phenol is TiNT CNT composite photocatalyst with acid treated HNO3 CNT. The maximum CNT loading in the TiNT CNT composite is 2 which has a performance for phenol elimination of 62. From the results obtained it can be stated that the composite design of Titania nanotubes TiNT and Carbon Nanotubes CNT has a promising potential as an alternative in treating phenol waste.
Depok: Fakultas Teknik Universitas Indonesia, 2018
D2376
UI - Disertasi Membership  Universitas Indonesia Library
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Athiek Sri Redjeki
Abstrak :
Metil ester asam lemak (Fatty Acid Methyl Ester = FAME) merupakan senyawa utama penyusun biodiesel dan bahan baku untuk surfaktan metil ester sulfonate (MES). Minyak kemiri sunan yang mempunyai kandungan minyak tinggi dalam setiap bijinya berpotensi menjadi bahan baku untuk produksi FAME. Kandungan asam lemak bebas (free fatty acid/FFA) dan asam lemak tak jenuh gandanya (asam α-eleostearat, C18: 3) yang tinggi dapat diminimalisir dengan esterifikasi dan reaksi adisi. Penelitian ini bertujuan menyintesis dan mengarakterisasi fotokatalis CuO/TiO2 untuk menurunkan kadar FFA dan jumlah asam lemak tak jenuh ganda (C18:3) dari minyak kemiri sunan dengan esterifikasi dan adisi secara simultan, mendapatkan kondisi operasi reaksi dan mendapatkan mekanisme reaksi prediksinya. Katalis CuO/TiO2 disintesis dengan cara impregnasi serbuk TiO2 P25 dengan larutan tembaga nitrat (Cu(NO3)2. 2H2O sebagai prekursor Cu dan dilanjutkan dengan kalsinasi. Hasil karakterisasi dengan (FESEM), Mapping, Energy Dispersive X-Ray (EDX), X-Ray Diffraction (XRD), Transmission electron microscopy (TEM) dan High resolution transmission electron microscopy (HRTEM) menunjukkan bahwa oksida tembaga (CuO) terdispersi dengan baik pada permukaan TiO2. Hasil X-Ray Photoelectron spectroscopy (XPS) menunjukkan bahwa Cu berada dalam bentuk senyawa CuO (Cu2+) sedangkan Ti dalam keadaan Ti4( TiO2.). Hasil karakterisasi ultra violet-vis diffuse reflectance spectroscopy (UV DRS) menunjukkan energi band gap dari semua sampel CuO/ TiO2 lebih kecil daripada TiO2 P25. Reaksi yang dilakukan dalam fotoreaktor di bawah paparan sinar UV ini mendorong terjadinya esterifikasi dan adisi FFA secara bersamaan. Penurunan FFA optimum pada kondisi kadar CuO/ TiO2 4%, waktu reaksi 4 jam, rasio molar minyak terhadap metanol 1:30, jumlah katalis 5% (b/b). Konversi FFA sekitar 59% dan kandungan akhir FFA masih lebih besar dari 2,5%.  Hasil karakterisasi gas chromatography mass spectroscopy (GCMS) menunjukkan bahwa reaksi adisi asam α-Eleostearat pada kondisi ini diperoleh konversi 100%. Meskipun kemampuan fotokatalis dalam penurunan FFA relatif rendah, namun penurunan ikatan rangkap asam α-Eleostearat (C18:3) sangat tinggi. Pengurangan ikatan rangkap ini merupakan sesuatu positif mengingat jumlah asam ±-Eleostearat dalam minyak kemiri sunan yang mencapai 41,8%.  Dengan adanya reaksi adisi yang berlangsung bersama dengan esterifikasi akan meningkatkan potensi minyak kemiri sunan sebagai bahan baku untuk FAME. Dalam disertasi ini, juga diusulkan mekanisme reaksi esterifikasi dan adisi secara bersamaan. ......Fatty acid methyl ester (FAME) is the main compound of biodiesel and raw material of methyl esther sulfonate (MES) surfactant. Kemiri sunan oil which has high oil content in its seed has high potential to be synthesized into FAME.  The high content of free fatty acid (FFA) and poly-unsaturated fatty acid (α-Eleostearic acid; C18:3) can be reduced by converting its FFA content through esterification and reducing its unsaturation number with an addition. The objectives of this research are to synthesize and characterized CuO/TiO2 photocatalyst for reducing the free fatty acid (FFA) and poly-unsaturated fatty acid content simultaneously, to study the operation condition of reaction and to study the reaction mechanism prediction. The CuO/TiO2 catalyst was synthesized by the impregnation of TiO2 P25 powder with copper nitrate solution as a precursor and followed by calcination. The Field emission scanning electron microscopy (FESEM), Mapping, Energy Dispersive X-Ray (EDX), X-Ray Diffraction (XRD), Transmission electron microscopy (TEM) and High resolution transmission electron microscopy (HRTEM) results showed that Copper oxide was highly dispersed on the TiO2 surface. The X-Ray photoelectron spectroscopy (XPS) result showed that Cu is in the state of CuO (Cu2+) while Ti is in Ti4 (TiO2). The ultra violet-vis diffuse reflectance spectroscopy (UV-DRS) results shows that the energy band gap of CuO/TiO2 samples were lower than TiO2 P25. It was found that reaction in the presence of CuO/TiO2 in a photoreactor under UV irradiation can perform esterification and addition reaction of the FFA, simultaneously. The optimum reduction of the FFA was under condition of 4% loading CuO/TiO2, 4 hours reaction time, 30:1 (mole/mole) metanol to oil ratio, 5% (w/w) catalyst amount. The conversion of  FFA was at around 59% and the final FFA content still more than 2.5%. The gas chromatogram mass spectroscopy (GCMS) results showed that the addition reaction of α-Eleostearic acid simultaneously occured at 100% conversion.  Although the photocatalyst performance in  FFA reduction was relatively  low, but double bond reduction of α-Eleostearic acid (C18:3) was very high. The reduction of multiple double bond is consideres as positive poin due to the amount of α-Eleostearic acid is very high (about 41,8%). The addition occurred with esterification simultaneously will increase the potency of kemiri sunan oil as a FAME raw material.  The simultaneous esterification and addition reactions mechanism has been proposed.
Depok: Fakultas Teknik Universitas Indonesia, 2021
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UI - Disertasi Membership  Universitas Indonesia Library