Etty Marti Wigayati
Pusat Penelitian Fisika – LIPI Kawasan Puspiptek, Serpong, Tangerang

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ANALISIS PENGARUH MECHANICAL MILLING MENGGUNAKAN PLANETARY BALL MILLING TERHADAP STRUKTUR KRISTAL DAN STRUKTUR MIKRO SENYAWA LIBOB Wigayati, Etty Marti; Purawiardi, Raden Ibrahim
Jurnal Sains Materi Indonesia Vol 16, No 3: APRIL 2015
Publisher : Center for Science & Technology of Advanced Materials - National Nuclear Energy Agency

Show Abstract | Download Original | Original Source | Check in Google Scholar | DOI: 10.17146/jsmi.2015.16.3.4230

Abstract

ANALISIS PENGARUH MECHANICAL MILLING MENGGUNAKAN PLANETARY BALL MILLING TERHADAP STRUKTUR KRISTAL DAN STRUKTUR MIKRO SENYAWA LiBOB. Telah dilakukan pembuatan senyawa Lithium bis Oksalat Borat (LiBOB) dari bahan baku LiOH, asam oksalat dan asam borat dengan metode reaksi padat padat. Serbuk yang dihasilkan dilanjutkan penghalusan menggunakan planetary ball milling dengan durasi milling di buat bervariasi (4 jam, 5 jam, 6 jam, 10 jamdan 13 jam). Serbuk LiBOB yang dihasilkan dianalisis menggunakan X-Ray Diffractometer (XRD) untuk mengetahui fasa yang terbentuk, struktur kristal dan ukuran kritalitnya. Hasil identifikasi senyawa LiBOB dengan XRD berupa pola difraksi kemudian dianalisismenunjukkan terbentuknya 2 fasa yaitu fasa LiB(C2O4)2 dan fasa LiB(C2O4)2.(H2O) dengan sistem kristal orthorhombic. Kerapatan atom paling kecil pada senyawa LiBOB dengan durasi milling 5 jam dan volum unit sel paling besar pada senyawa LiBOB dengan durasi milling 10 jam. Diameter ukuran kristalit berubah seiring dengan durasi milling, sedang regangan kisi terendah pada durasi milling 4 jam dan tertinggi pada durasi milling 5 jam. Durasi milling 5 jam adalah paling bagus dimana pada fasa ini memberikan ruang paling besar pada tiap unit sel dan regangan kisi paling besar sehingga dapat memudahkan ruang gerak transfer ion Li pada baterai Lithium. Senyawa LiBOB hasil sintesis mempunyai sistem kristal yang teratur. Tingkat keteraturan kristal yang dihasilkan ditunjukan dengan perhitungan indeks kristalinitas yang tinggi.
Pengaruh Penambahan LiClO4 pada Pembuatan Komposit Anoda Grafit Bermatrik Polimer Prihandoko, Bambang; Wigayati, Etty Marti; Nurhayati, Nurhayati
Jurnal Fisika dan Aplikasinya Vol 3, No 1 (2007)
Publisher : Jurnal Fisika dan Aplikasinya

Show Abstract | Download Original | Original Source | Check in Google Scholar | Full PDF (722.91 KB) | DOI: 10.12962/j24604682.v3i1.992

Abstract

Telah dilakukan penelitian tentang pengaruh penambahan LiClO4 pada pembuatan komposit anoda grafit bermatrik polimer. Komposit anoda grafit digunakan sebagai komponen baterai lithium. Komposit bermatriks polimer ini berbentuk lembaran tipis dan dapat diperoleh melalui proses pembuatan dengan metode tape casting yang menggunakan perangkat doctor blade. Ketipisan komposit anoda yang diperoleh berkisar sekitar 60 μm. Penambahan LiClO4 dilakukan dalam 0, 2, 4, 6, 8 dan 10%berat dari campuran bahan keramiknya, yaitu serbuk grafit dan karbon black. Penambahan ini ternyata tidak mempengaruhi pada proses pembuatan dan hasil lembarannya tetap tipis dan merata, tidak ada penggumpalan. Hasil pengamatan XRD menunjukkan keberadaan lithium perklorat hidrat yang disebabkan adanya reaksi antara uap air dan LiClO4. Komposisi nilai konduktivitaslistrik bernilai optimum diperoleh pada penambahan 4% LiClO4. Konduktivitas listrik komposit anoda meningkat dengan penambahan LiClO4 dan mencapai nilai optimum pada penambahan 4% LiClO4 yaitu sebesar 3,8 x 10−5 Scm−1 untuk nilai konduktivitas total dan sebesar 9,5 x 10−5 Scm−1 untuk nilai konduktivitas elektron.
Microstructure Analysis of Synthesized LiBOB Wigayati, Etty Marti; Ratri, Christin Rina; Purawiardi, Ibrahim; Rohman, Fadli; Lestariningsih, Titik
Indonesian Journal of Chemistry Vol 15, No 3 (2015)
Publisher : Universitas Gadjah Mada

Show Abstract | Download Original | Original Source | Check in Google Scholar | Full PDF (484.528 KB) | DOI: 10.22146/ijc.21191

Abstract

Lithium bis (oxalate) borate or LiBOB is an active material used as the electrolyte for lithium battery application. LiBOB (LiB(C2O4)2) powder was prepared from LiOH, H2C2O4 and H3BO3. 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 C4LiBO8 and LiB(C2O4)2.H2O, 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 m2/g, 0.4252 cm3/g, and 19.2 nm respectively.
PEMBUATAN BATAKO DARI ABU HASIL INSINERASI SAMPAH DOMESTIK DAN KARAKTERISASINYA Wigayati, Etty Marti; Muljadi, Muljadi
Jurnal Ecolab Vol 2, No 2 (2008): Ecolab : Jurnal Pemantauan Kualitas Lingkungan
Publisher : Pusat Penelitian dan Pengembangan Kualitas dan Laboratorium Lingkungan (P3KLL)

Show Abstract | Download Original | Original Source | Check in Google Scholar | DOI: 10.20886/jklh.2008.2.2.59-65

Abstract

Garbage problems are increasing day by day. Garbage problems may generate environmental pollution problemswith its impact are continued to be increased. One of the technology to destroy the garbage is by incinerator. Thestudy was trying to reuse the ash resulted from the incineration of garbage by incinerator which have an addedvalue. The ash composition was similar as clay, so the ash could be used as a raw material for making batako whichare the weight ratio between sand and comment was 3:1. Some of sand was substituted by ash from incinerator withcompositions of 0%, 10%, 20%, 25%, and 30%. All the raw materials were homogenously mixed, and then wereformed by casting and were dried in open air variation of time between 7 days and 28 days. The resulting dried batakowere characterized for its density as indicated the decreasing density was in line with the increasing of ash assubstituted and the drying time of 28 days gave result the bigger one. The porosity value decreased along with theash content and giving the smallest one after drying 28 days. The water absorption value will decreased along withthe increasing ash content and the longer time of drying process. The bending and compressive strength value weregrowing larger with increasing ash content, and by giving 25% ash, the compressive strength value became stabilized.Comparing to the existing batako market, batako using incinerator ash gave better quality.
PEMBUATAN NANOPAR TIKEL LixMn2O4 Wigayati, Etty Marti
Teknologi Indonesia Vol 32, No 2 (2009)
Publisher : LIPI Press

Show Abstract | Download Original | Original Source | Check in Google Scholar | DOI: 10.14203/jti.v32i2.10

Abstract

LixMn2O4 nanoparticle has been prepared using Li2CO3 and MnO2 as starting materials. Firstly, Li2CO3 and MnO2 were mixed using solid state reaction, then the powder was calcinated at 700oC and sintered at 800oC. The resulted pouder was characterized using SEM, XRD, and EIS (Electrochemical Impedance Spectroscopy). Henceforth, LixMn2O4 powder was processed into nanoparticle size through milling process using PBM (Planetary Ball Milling) for 80 hour and ultrasonificator with power of 300 watt for 2 hour. The characterization was conducted again using SEM, XRD, PSA and EIS. The result shows that there is no diffraction pattern change after the milling process. Examination using SEM shows particle changes from needles to round shapes with smaller sizes. Diffraction analyzes using Rietveld method results in lattice parameter of 8.23454 , cell unit volume of 558.3647 3 and the crystal structure is cubic with space group of Fd-3m. The particle size of the final product is analyzed using Particle Size Analyzer (PSA) which results in the value of 178 nm in average diameter. The measurement of electrical impedance gives values of 2 M ohm (before milling) and 8 M ohm (after milling).
SINTESIS LiBOB DAN ANALISA STRUKTUR KRISTALNYA [Synthesis and Analysis Crystalline Structure LiBOB] wigayati, etty marti
Metalurgi Vol 30, No 2 (2015): Metalurgi Vol.30 No.2 Agustus 2015
Publisher : Pusat Penelitian Metalurgi dan Material - LIPI

Show Abstract | Download Original | Original Source | Check in Google Scholar | Full PDF (571.753 KB) | DOI: 10.14203/metalurgi.v30i2.28

Abstract

Litium Bis(Oksalato) Borat atau LiBOB merupakan garam Lithium yang saat ini mulai dikembangkan sebagai elektrolit alternatif untuk baterai Li-Ion. Elektrolit padat LiBOB dianggap lebih ramah lingkungan, LiBOB juga memiliki stabilitas panas yang cukup tinggi yakni sebesar 302 °C. Penelitian ini bertujuan untuk mensintesis LiBOB kemudian untuk mengetahui struktur kristalnyadan untuk mengetahui durasi sintering yang optimum. Sintesis LiBOB (Lithium bis oksalat borat)dilakukan melalui metoda solid state reaction. Bahan awal dicampur hingga homogen. Kalsinasi dilakukan pada temperatur 120 °C,ditahan selama 2 jam dilanjutkan dengan sintering pada temperatur 240 °C dengan penahanan dilakukan secara bervariasi yaitu 2 jam, 3 jam, dan 4 jam. Untuk mengetahui fasa yang terbentuk dilakukan karakterisasi dengan XRD. Dari hasil analisis XRD dapat diidentifikasi fasa yang terjadi pada waktu penahanan 2 jam masih muncul fasa dari bahan awal, LiBOB hidrat dan beberapa fasa impuritas. Pada waktu penahanan 3 jam terbentuk fasa LiBOB hidrat dan H3BO3. Pada penahanan 4 jam muncul fasa LiBOB dan LiBOB hidrat serta beberapa fasa impuritas. Sampel dengan penahanan 4 jam merupakan sampel yang paling optimum mendekati karakteristik kristal LiBOB dan LiBOB Hidrat pada sampel LiBOB komersial. Struktur kristal LiBOB yang terbentuk adalah orthorombik dengan nilai a, b, dan c sebesar 5.74 Å, 6,79 Å, dan 14,45 Å dengan sudut α = β = γ = 90°, grup ruangPnma (62), serta nilai FoM 1,386. Sementara struktur kristal LiBOB Hidrat juga orthorombik namun dengan nilai a, b, dan c sebesar 16,119 Å, 15,913 Å, dan 5,6182 Å dengan sudut α = β = γ = 90°, grup ruang Pbca (61), serta nilai FoM 0,824. AbstractLithium Bis ( Oxalato ) Borate(LiBOB) as lithium salt that is currently being developed as an alternativeelectrolytes for Li - Ion battery. LiBOB electrolyte is considered more environmentally friendly, LiBOB alsohave a fairly high heat stability which is equal to 302 ºC.This research aims to synthesize LiBOB thentodetermine the crystal structure and the optimum duration of sintering.At present work, the synthesis ofLithium Bisoxalato Borate (LiBOB) was done by solid-state reaction method. The raw materials was mixedhomogeneously. These samples were calcinated at 120 ºC for about 2 hours then sintered at 240 ºC withvarious durations (2, 3, and 4 hours). XRD characterization was done for identifying phases. From XRDinterpretation, there are LiBOB Hydrate and other impurities at two-hour sintered sample. There are LiBOBHydrate and H3BO3 at three-our sintered sample. There are LiBOB, LiBOB Hydrate, and other impurities atfour-hour sintered sample. The sample with 240 ºC/4 hour parameter is the most optimum sample based onthe convergention to the LiBOB and LiBOB Hydrate phases at standard commercial LiBOB sample (SigmaAldric). The crystal system of the LiBOB phase is orthorombic with lattice parameters a = 5.74 Å, b = 6.79Å, c = 14.45 Å, α = β = γ = 90º, space groupPnma (62), and FoM 1.386. On the other hand, the crystal systemof LiBOB Hydrate phase is also orthorombic with lattice parameters a = 16.119 Å, b = 15.913 Å, c = 5.6182Å, α = β = γ = 90º, space group Pbca (61), and FoM 0.824.