Sintesis Sol-Gel dan Karakterisasi Struktur Padatan FeF3 dengan Difraksi Sinar-X
DOI:
https://doi.org/10.53342/pharmasci.v4i1.127Abstract
ABSTRAK
Material FeF3 dapat diaplikasikan dalam berbagai bidang diantaranya sebagai material katoda untuk baterai ion litium dan katalis heterogen pada beberapa reaksi yang melibatkan sisi asam. Sintesis FeF3 dapat dilakukan melalui beberapa cara, salah satunya dengan metode sol-gel. Di dalam proses sol-gel adanya agen gelasi dapat mengontrol porositas dan sifat keasaman katalis. Pada penelitian ini dipilih agen gelasi dari senyawa alkohol yaitu metanol dan etanol. Masing-masing padatan yang telah disintesis kemudian dikarakterisasi struktur padatannya dengan difraksi sinar-X. Hasil penelitian menunjukkan bahwa padatan FeF3 telah berhasil disintesis melalui metode sol gel dengan agen gelasi yang berbeda yaitu metanol dan etanol yang masing-masing dituliskan sebagai FeF3(me) dan FeF3(et). Karakterisasi struktur padatan FeF3 menggunakan difraksi sinar-X menghasilkan difraktogram yang sesuai dengan PDF No. 85-0481 dan data ICSD kode 016671 yang memiliki
struktur rhombohedral dengan space group R-3cR dan panjang kisi kristal sebesar a = b = c = 5,362 Å dengan sudut α = β = γ = 57,99°. Struktur kristal FeF3 disusun oleh ion Fe3+ dengan jari-jari 0,384 Å dan ion F- dengan jari-jari 0,798 Å dengan tipe ikatan ionik. Rasio besarnya kristalinitas FeF3(et) dibandingkan dengan kristalinitas
FeF3(me) sebesar 5:4.
Kata kunci: FeF3, sintesis sol-gel, difraksi sinar-X, struktur padatan.
FeF3 material can be applied in various fields including as cathode material for lithium ion batteries and heterogeneous catalysts in some reactions involving the acid side. Synthesis of FeF3 can be done in several ways, one of them is the sol-gel method. In the sol-gel process the gelation agent can control the porosity and acidity of the catalyst. In this study, gelation agents were selected from alcohol compounds, namely methanol and ethanol. The solids that has been synthesized was then solid structure characterized by X-ray diffraction. The results showed that FeF3 solids were successfully synthesized through the sol-gel method with different gelation agents, namely methanol and ethanol, each of which was written as FeF3(me) and FeF3(et). Characterization of the solid structure of FeF3 using X-ray diffraction produces a diffractogram according to the PDF No. 85-0481 and ICSD data code 016671 which has a rhombohedral structure with space group R-3cR and
crystal lattice length of a = b = c = 5.362 Å with an angle α = β = γ = 57.99°. The crystal structure of FeF3 is composed by Fe3+ ions with radius 0.384 Å and F- ions with radius 0.798 Å with ionic bond types. The ratio of the crystallinity of FeF3(et) compared to the crystallinity of FeF3(me) is 5:4.
Keywords: FeF3, sol-gel synthesis, X-ray diffraction, solid structur.
References
Chen C, Xu X, Chen S, Zheng B, Shui M, Xu L, et al. The preparation and characterization of iron fluorides polymorphs FeF3·0.33H2O and β- FeF3∙3H2O as cathode materials for
lithium-ion batteries. Materials Research Bulletin. 2015: 64(2015): 187-193.
Guo Y. Novel nanoscopic FeF3–based materials: synthesis, characterisation, and catalytic applications (disertasi). Jerman: Humboldt-Universität zu Berlin;
Surasani R, Kalita D, Rao AVD, Yarbagi K, Chandrasekhar, KB. FeF3 as a novel catalyst for the synthesis of polyhydroquinoline derivatives via unsymmetrical Hantzsch reaction. J. Fluorine Chem. 2012: 135(1): 91-96.
Murthy JK, Gross U, Rüdiger S, dan Ünveren E. Synthesis and Characterization of Chromium (III)-doped Magnesium Fluoride Catalysts. Applied Catalysis A: General, 2004. 282(1-2): 85-91.
Valerie NN, Murwani IK. MgF2 as Catalyst and Support on Phenol Acylation. Oral presentation in The First International
Seminar on Science and Technology (ISSTEC); 24 Januari 2009; Yogyakarta, Indonesia. Indonesia : Universitas Gadjah Mada; 2009.
Ali G, Lee JH, Chang W, Cho BW, Jung HG, Nam KW, et al. Lithium Intercalation Mechanism into FeF3·0.5H2O As A Highly Stable Composite Cathode Material. Scientific Reports. 2017: 7:
Murwani IK, Kemnitz E, Skapin T, Amiry MN, Winfield JM. Mechanism Investigation of Hydrodechlorination of
,1,1,2-Tetrafluorodichloroethane on Metal Fluoride-Supported Pd and Pd. Catalysis Today. 2004: 88(34): 153–168.
A’yuni Q. Sintesis Katalis MgF2 Metode Sol-Gel dengan Gelating Agent Etanol dan Etilen Glikol serta Kinerjanya pada Reaksi Asetilasi Gliserol, Surabaya: Kimia ITS; 2015.
Wojciechowska M, Zieliński M dan Pietrowski M. MgF2 as A NonConventional Catalyst Support. Journal of Fluorine Chemistry. 2003. 120(1): 1–11.
López T, Gómez O, Navaro A, RamÃrez-SolÃs E, Sánchez-Mora S, Castillo E, et al. SolGel Ru/SiO2-Catalyst: Theoretical and
Experimental Determination of the Ruin-Silica Structure. J. Catal. 1993:141(1): 11–23.
Murthy JK, Groß U, Rüdiger S, Ünveren E Kemnitz E. FeF3/MgF2: Novel Lewis Acidic Catalyst Systems. Applied
Catalysis A: General. 2004: 278(1): 133–138.
Wuttke S, Coman SM, Kröhnert J, Jentoft FC, Kemnitz E. Sol–Gel Prepared Nanoscopic Metal Fluorides – a NewClass of Tunable. Catalysis. 2010:152(1-4): 2–10.
Murwani IK, Scheurell K, Kemnitz E. Liquid phase oxidation of ethylbenzene on pure and metal doped HS-AlF3.
Catalysis Communications. 2008: 10(2): 227–231.
Rayalu SS, Udhoji JS, Meshram SU, Naidu RR, Devotta S. Estimation of crystallinity in flyash-based zeolite-A
using XRD and IR spectroscopy. Current Science. 2005: 89 (12): 2147-2151.
Zhang G, Liu M. Preparation of Nanostructured Tin Oxide Using A SolGel Process Based on Tin Tetrachloride and Ethylene Glycol. Journal of Materials Science. 1999: 34(13): 3213–3219.
