Indones. J. Chem., 2015, 15 (3), 242 - 247 Etty Marti Wigayati et al. 242 * Corresponding author. Tel/Fax : +62-21-7560570/7560556 Email address : etty001@lipi.go.id MICROSTRUCTURE ANALYSIS OF SYNTHESIZED LiBOB Etty Marti Wigayati * , Christin Rina Ratri, Ibrahim Purawiardi, Fadli Rohman, and Titik Lestariningsih Research Center for Physics, Indonesian Institute of Sciences, Kawasan Puspiptek Serpong Gd. 442 Tangerang Selatan 15314, Banten Indonesia Received March 3, 2015; Accepted June 4, 2015 ABSTRACT Lithium bis (oxalate) borate or LiBOB is an active material used as the electrolyte for lithium battery application. LiBOB (LiB(C 2 O 4 ) 2 ) powder was prepared from LiOH, H 2 C 2 O 4 and H 3 BO 3 . The employed method was solid state reaction. LiBOB powder produced from the reaction was then observed using SEM and TEM. Surface area was analyzed using Quantachrome Nova 4200e. From the analysis analyzed using XRD to identify the resulting phases, crystal structure, and crystallite size. The functional groups were analyzed using FT-IR. The particle morphology was result, it was seen that the resulted phases were C 4 LiBO 8 and LiB(C 2 O 4 ) 2 .H 2 O, the crystal structure was orthorhombic with space group Pbca and Pnma. From the particle morphology observation it was shown that micro pores were created irregularly. When the observation was deepened, nanopores with elongated round shape were seen within the micropores. The pore size was approximately 50–100 nm. The surface area, total pore volume, and average pore diameter of LiBOB powder was 88.556 m 2 /g, 0.4252 cm 3 /g, and 19.2 nm respectively. Keywords: phase; crystal structure; crystallite size; functional group; nanopores particle morphology ABSTRAK LiBOB (Lithium bis oksalat borat) merupakan bahan aktif yang dapat dipergunakan untuk elektrolit pada baterai Lithium. Serbuk LiBOB (LiB(C 2 O 4 ) 2 ) dibuat dari bahan baku LiOH, H 2 C 2 O 4 dan H 3 BO 3 . Metoda yang dipergunakan adalah solid state reaction. Serbuk LiBOB yang dihasilkan dianalisa menggunakan XRD untuk mengetahui fasa yang terbentuk, struktur kristal dan ukuran kristalitnya. Ikatan gugus fungsi dianalisa dengan FTIR. Morfologi partikel diamati dengan SEM dan TEM. Surface area dianalisis dengan alat Quantachrome Nova 4200e. Dari hasil analisis dapat diketahui bahwa fasa yang terbentuk adalah fasa C 4 LiBO 8 dan LiB(C 2 O 4 ) 2 (H 2 O), struktur kristal orthorhombic dengan space group Pbca dan Pnma. Pada pengamatan morfologi partikel dapat diketahui terbentuk rongga pori dalam ukuran mikro dengan bentuk tidak beraturan. Ketika pengamatan diperdalam lagi pada bagian rongga pori nampak terjadi nanopori dengan bentuk bulat sedikit memanjang. Ukuran pori berkisar 50-100 nm. Luas permukaan, volume pori total, dan rerata diameter pori dari serbuk LiBOB masing-masing adalah 88,556 m 2 /g, 0,4252 cm 3 /g, dan 19,2 nm. Kata Kunci: fasa; struktur kristal; ukuran kristalit; ikatan gugus; morfologi partikel nanopori INTRODUCTION Lithium bis(oxalato) borate (LiBOB) is a new lithium salt firstly proposed at 1999 by Lischka et al. [1-2] as a highly promising and advantageous electrolyte for rechargeable lithium-ion batteries. Thermal behavior of LiBOB is an interesting and important research subject especially concerning the safety of lithium-ion batteries. In the last few years, several researchers have published LiBOB-related scientific journals, particularly discussing thermal studies of LiBOB which showed excellent thermal stability up to 300 °C. Beyond this temperature, LiBOB would be decomposed into Li 2 CO 3 , B 2 O 3 , and CO 2 [3-5]. Another publication explained that LiBOB electrolyte dissolved in propylene carbonate (PC) solvent that showed has higher power capability compared to another lithium salts in similar solvent [6- 7]. It was also explained that the charge/discharge test of 0.7 M LiBOB in EC:EMC (1:1) solvent showed more superior performance compared to 1 M LiPF 6 in EC:EMC (1:1) solvent. LiBOB has higher stability and discharge capacity at high temperature [8]. In addition, LiBOB has distinctive physical properties such as hygroscopic and stable when it contacts with water. However, LiBOB solubility in the mixture of carbonate solvent to form liquid electrolyte was found to be relatively low compared to LiPF 6 , therefore microstructure observation of LiBOB powder is necessary. In this research, LiBOB powder was synthesized using solid state reaction method, and