SINTESIS DAN KARAKTERISASI Li4Ti5O12 YANG DILAPISI KARBON DENGAN METODE SOLID STATE REACTION UNTUK ANODA ION LITHIUM

Author(s):  
Lediliocza Lediliocza ◽  
Sitti Ahmiatri Saptari ◽  
Slamet Priyono

Telah dilakukan sintesis material anoda Li4Ti5O12 dilapisi karbon melalui metode solid state, dengan bahan baku LiOH H2O dan TiO2. sintesis dilakukan dengan variasi sumber karbon yaitu Super. P, Tapioka, dan karbon aktif Food grade. Prekursor Li4Ti5O12 disinter pada suhu 800o C selama 4 jam pada atmosfer udara bebas. Sedangkan proses pelapisan karbon dilakukan dengan milling basah dan sinter pada suhu 600o C selama 1 jam pada atmosfer N2. Karakterisasi yang dilakukan meliputi analisa untuk melihat perbedaan performa elektrokimia pada variasi sumber karbon yang digunakan, diantaranya analisa XRD (X-ray Diffraction) untuk mengetahui pembentukan fasa Li4Ti5O12, FESEM ( Field Emission Scanning Electron Microscopy) untuk menganalisa morfologi yang terbentuk, dan untuk mengetahui performa elektrokimia dilakukan pengujian Cyclic voltammetry, charge-discharge dan Electrochemical Impedance Spectroscopy (EIS). Hasil karaktrisasi terbentuk fasa Lithium titanium oxide (Li4Ti5O12) sebesar 96,1% dan fasa rutile (TiO2) sebesar 3,1%. Hasil karakterisasi FE-SEM menunjukan morfologi penyebaran karbon pada anoda Li4Ti5O12/C dengan sumber karbon Super P, paling homogen dbandingkan dengan anoda Li4Ti5O12/C dengan sumber karbon Tapioka kemudian anoda Li4Ti5O12/C dengan sumber karbon food grade. Performa elektrokimia yang dihasilkan Li4Ti5O12/C dengan sumber karbon Tapioka memiliki nilai konduktivitas elektronik dan konduktivitas ionik paling besar, dan menunjukan difusi ion lithium yang sangat kecil, namun memiliki nilai koefesien difusi 2,54 × 10−13 cm-2 s-1 mendekati besar koefesien difusi Li4Ti5O12/C (Sp) sebesar 2,61 × 10−13 cm-2 s1, serta memiliki nilai kapasitas discharge 161.05 mAh/g, mendekati nilai kapasitas discharge Li4Ti5O12/C (Sp) sebesar 167.84 mAh/g. 

2009 ◽  
Vol 610-613 ◽  
pp. 498-501
Author(s):  
Guang Chuan Liang ◽  
Xiao Ke Zhi ◽  
Xiu Qin Ou ◽  
Li Wang

Mg2+ doped LiFePO4 was synthesized from Li3PO4, FeSO4 and MgSO4 by a hydrothermal synthesis at 150 °C(Li1-xMgxPO4, x=0.00, 0.01,0.02,0.04,0.06). The samples were characterized with X-ray diffraction (XRD), scanning electron microscopy (SEM) and charge-discharge test. The results showed that Mg2+ dissolved in the LiFePO4 lattice. When the content is in the range of 0 to 6 mol%, Mg2+ caused the shrinkage of LiFePO4 cell volume. The capacity of doped and undoped samples at low discharging rate was similar, about 145mAhg-1 for 0.2C. But the sample doped with 2-4 mol% Mg2+ has higher capacity and longer cycle lifetime than the undoped one at 5C.


2014 ◽  
Vol 215 ◽  
pp. 158-162
Author(s):  
Liudmila E. Bykova ◽  
V.G. Myagkov ◽  
I.A. Tambasov ◽  
O.A. Bayukov ◽  
Victor S. Zhigalov ◽  
...  

A simple method for obtaining ZnO-Fe3O4 nanocomposites using solid-state reaction Zn + 3Fe2O3 ZnO + 2Fe3O4 is suggested. An analysis of the characteristics and properties of ZnO-Fe3O4 nanocomposites was carried out by a combination of structural and physical methods (X-ray diffraction, scanning electron microscopy, photoelectron spectroscopy, Mössbauer measurements, X-ray fluorescent analysis, and magnetic measurements). The magnetization of the hybrid ZnO-Fe3O4 films is equal to 440 emu/cm3. The resulting Fe3O4 nanoparticles are surrounded by a ZnO shell and have sizes ranging between 20 and 40 nm.


2020 ◽  
Vol 31 (8) ◽  
pp. 1367-1384 ◽  
Author(s):  
C Karthikeyan ◽  
R Dhilip Kumar ◽  
J Anandha Raj ◽  
S Karuppuchamy

Metal sulfides received key interest as an electrode material for storage and conversion of energy. Here, the novel nanostructured N17S18 and (CoNi)3S4 materials were synthesized via one-step hydrothermal method, and the synergistic effect of metal ions and electrochemical properties was investigated. A new and simple solution growth technique was employed in this work. The prepared nanopowders were characterized by X-ray diffraction, Fourier transform infrared spectroscopy, field emission scanning electron microscopy, energy-dispersive X-ray spectroscopy techniques. The X-ray diffraction analysis of the prepared nanopowder revealed the formation of cubic phase cobalt nickel sulfides (CoNi)3S4 and hexagonal phase nickel sulfides (Ni17S18). Scanning electron microscopy analysis display fibrous, flakes and sheet-like morphology for CoxSx, N17S18 and (CoNi)3S4, respectively. Fibrous and sheet-like morphology exhibits higher electrochemical performance in supercapacitors. The electrochemical behavior of the amorphous CoxSx, crystallite Ni17S18 and (CoNi)3S4 modified electrodes was investigated using electrochemical impedance spectroscopy, cyclic voltammetry and galvanostatic charge–discharge techniques. The specific capacitance of 57 F/g and 31 F/g were obtained for the amorphous CoxSx and crystalline (CoNi)3S4 powder, respectively. Amorphous CoxSx modified electrode retains 76% of initial capacitance after 1000 repeated cycling process. These results of this study suggest that the CoxSx and crystalline (CoNi)3S4 are appropriate materials for supercapacitor applications.


Materials ◽  
2021 ◽  
Vol 14 (10) ◽  
pp. 2557
Author(s):  
Chloé Cherpin ◽  
Derek Lister ◽  
Frédéric Dacquait ◽  
Lihui Liu

Spinel ferrite compounds continue to receive a lot of attention due to their unique properties. Among the numerous synthesis routes existing, the solid-state method was applied for the production of nickel ferrite, by introducing the use of a quartz vial. A mixture of nickel oxide (NiO) and hematite (Fe2O3) was ground and vacuum-sealed in the vial and different thermal treatment programs were tested. The resulting particles were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and Raman spectroscopy. For temperatures, below 1000 °C, the solid-state reaction is not complete as nickel oxide (NiO) and hematite (Fe2O3) are still present. The reaction time is a decisive parameter for the morphology of the particles obtained. If, for different reaction times, the particle size distribution is always between 0.3 and 1.7 µm, a longer reaction time leads to the formation of dense, interconnected clusters of particles. Optimal parameters to synthesize a pure phase of spherical nickel ferrite were sought and found to be a reaction temperature of 1000 °C for 72 h.


2012 ◽  
Vol 151 ◽  
pp. 310-313
Author(s):  
Jenn Sen Lin ◽  
Teng Chin Yu ◽  
Cheng Hsing Hsu ◽  
Ci Jie Huang ◽  
His Wen Yang

The microstructure properties of the perovskite Bi0.5Na0.5TiO3-BaZrO3 ceramics were prepared with the conventional solid-state route have been investigated. The resultant microstructure properties were analyzed based upon the densification, the X-ray diffraction patterns and scanning electron microscopy. The correlation between the microstructures and the sintering temperature was also examined.


2012 ◽  
Vol 535-537 ◽  
pp. 797-800
Author(s):  
Liang Luo ◽  
Yan Jun Zhu ◽  
Ling Ling Song ◽  
Xiao Bo Zhang

A facile one-pot hydrothermal method has been developed for synthesis of porous and non-porous BaTiO3 ceramics using Ba(OH)2.8H2O, BaCO3 as barium source. In this paper, we research the effect of different barium source on the nanostructure of BaTiO3 ceramics in a solid state reaction, and the results indicated that the two different morphologies of BaTiO3 ceramics can be easily prepared by using these two different barium source. The phase composition and morphology of the as-obtained products were investigated by X-ray diffraction and field emission scanning electron microscopy (SEM).


2014 ◽  
Vol 900 ◽  
pp. 242-246 ◽  
Author(s):  
Xing Ling Lei ◽  
Hai Yan Zhang ◽  
Yi Ming Chen ◽  
Wen Guang Wang ◽  
Zi Dong Huang ◽  
...  

LiFePO4/graphene composites were prepared via a simple hydrothermal method. The as-prepared LiFePO4/graphene composites were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), galvanostatic charge-discharge test, cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) tests. The lithium-ion batteries using LiFePO4/graphene composites as cathode material exhibited a discharge capacity of 165 mAh/g, which was 97% of the theoretical capacity of 170 mAh/g.


Author(s):  
Vicki L. Baliga ◽  
Mary Ellen Counts

Calcium is an important element in the growth and development of plants and one form of calcium is calcium oxalate. Calcium oxalate has been found in leaf seed, stem material plant tissue culture, fungi and lichen using one or more of the following methods—polarized light microscopy (PLM), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and x-ray diffraction.Two methods are presented here for qualitatively estimating calcium oxalate in dried or fixed tobacco (Nicotiana) leaf from different stalk positions using PLM. SEM, coupled with energy dispersive x-ray spectrometry (EDS), and powder x-ray diffraction were used to verify that the crystals observed in the dried leaf with PLM were calcium oxalate.


Author(s):  
Howard S. Kaufman ◽  
Keith D. Lillemoe ◽  
John T. Mastovich ◽  
Henry A. Pitt

Gallstones contain precipitated cholesterol, calcium salts, and proteins. Calcium (Ca) bilirubinate, palmitate, phosphate, and carbonate occurring in gallstones have variable morphologies but characteristic windowless energy dispersive x-ray (EDX) spectra. Previous studies of gallstone microstructure and composition using scanning electron microscopy (SEM) with EDX have been limited to dehydrated samples. In this state, Ca bilirubinates appear as either glassy masses, which predominate in black pigment stones, or as clusters, which are found mostly in cholesterol gallstones. The three polymorphs of Ca carbonate, calcite, vaterite, and aragonite, have been identified in gallstones by x-ray diffraction, however; the morphologies of these crystals vary in the literature. The purpose of this experiment was to study fresh gallstones by environmental SEM (ESEM) to determine if dehydration affects gallstone Ca salt morphology.Gallstones and bile were obtained fresh at cholecystectomy from 6 patients. To prevent dehydration, stones were stored in bile at 37°C. All samples were studied within 4 days of procurement.


2016 ◽  
Vol 5 (1) ◽  
pp. 6
Author(s):  
Budi Setiawan ◽  
Erizal Zaini ◽  
Salman Umar

Sebuah penelitian tentang sistem dispersi padat dari asiklovir dengan poloxamer 188 telah dilakukan formulasi dengan pencampuran secara fisika dengan rasio 1 : 1, 1 : 3, 1 : 5 dan dispersi padat 1 : 1, 1 : 3, 1 : 5 dan penggilingan 1:1 sebagai pembanding. Dispersi padat dibuat menggunakan metode pencairan (fusi), yang digabung dengan poloxamer 188 pada hotplate kemudian asiklovir dimasukkan ke dalam hasil poloxamer 188 lalu di kocok hingga membentuk masa homogen. Semua formula yang terbentuk termasuk asiklovir poloxamer 188 murni dianalisis karakterisasinya dengan Differential Thermal Analysis (DTA), X-ray Diffraction, Scanning Electron Microscopy (SEM), dan Fourier Transform Infrared (FTIR), kemudian pengambilan dilakukan  (penentuan kadar) mengunakan spektrofotometer UV pada panjang gelombang 257,08 nm dan uji laju disolusi dengan aquadest bebas CO2 menggunakan metode dayung. Hasil pengambilan  (penentuan kadar) menunjukkan bahwa semua formula memenuhi persyaratan farmakope Amerika edisi 30 dan farmakope Indonesia edisi 4 yaitu 95-110%. Sedangkan hasil uji laju disolusi untuk campuran fisik 1: 1, dan dispersi padat 1: 1, dan penggilingan 1: 1 menunjukkan peningkatan yang nyata dibandingkan asiklovir murni. Hal ini juga dapat dilihat dari hasil perhitungan statistik  menggunakan analisis varian satu arah  SPSS 17.


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