One pot and large-scale synthesis of nanostructured metal sulfides: Synergistic effect on supercapacitor performance

2020 ◽  
Vol 31 (8) ◽  
pp. 1367-1384 ◽  
Author(s):  
C Karthikeyan ◽  
R Dhilip Kumar ◽  
J Anandha Raj ◽  
S Karuppuchamy
Keyword(s):  
Electron Microscopy ◽  
Scanning Electron Microscopy ◽  
Synergistic Effect ◽  
Large Scale ◽  
Electrochemical Impedance ◽  
Metal Sulfides ◽  
Cubic Phase ◽  
X Ray Diffraction ◽  
X Ray ◽  
Scanning Electron

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.

scholarly journals Synthesis and characterization of graphene oxide flakes for transparent thin films

2021 ◽  
Vol 22 (3) ◽  
pp. 595-601
Author(s):  
R.G. Abaszade ◽  
S.A. Mamedova ◽  
F.G. Agayev ◽  
S.I. Budzulyak ◽  
O.A. Kapush ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Scanning Electron Microscopy ◽  
Graphene Oxide ◽  
Indium Tin Oxide ◽  
Electromagnetic Interference ◽  
Large Scale ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Scanning Electron

We have synthesized large scale, thin, transparent graphene oxide (GO) flakes by Hummer’s method and investigated their suitability for fabrication of transparent nanocomposites. The GO flakes were comprehensively characterized by X-ray diffraction, Scanning Electron Microscopy (SEM), Energy Dispersive X-ray analysis (EDX), Raman spectroscopy and Differential Scanning Calorimetry (DSC). X-ray diffraction displayed the peak of graphene oxide at 9°degree, which is characteristic peak of GO in agreement with the literature results. Scanning Electron Microscopy images revealed that thin, transparent, flake form GO with 14,8 µm lateral size and 0,31µm thickness were synthesized. The comparison with literature results show that for the first time, our group could synthesize large scale, thin and more transparent GO flakes by simple Hummer’s method using simple dispersed graphite. EDX measurements indicate the formation of layered structure with oxygen containing functional groups. The intensity ratio between D and G peaks in the Raman spectra proves that less defective GO flakes have been synthesized. The solution ability of the synthesized material indicate that high quality GO flakes were synthesized, which make them effective soluble material due to oxygen containing groups formed on the graphene plane during synthesis process.DSC results shows that these flakes are thermally stable till 200°C.  Due to high solubility properties, large scale and transparency they can be very useful in fabrication of high optical transparent nanocompoties for replacement indium tin oxide transparent conductors in solar panels, biomedical applications and microwave absorbers for electromagnetic interference (EMI) environmental protection.

Study on the Structure and Morphology of CexZr(1-x)O2 Mixed Oxides

2014 ◽  
Vol 938 ◽  
pp. 46-51 ◽  
Author(s):  
M. Nazri Abu Shah ◽  
S. Hanim Md Nor ◽  
Kamariah Noor Ismail ◽  
Abdul Hadi
Keyword(s):  
Electron Microscopy ◽  
Scanning Electron Microscopy ◽  
Mixed Oxides ◽  
Average Crystallite Size ◽  
Cubic Phase ◽  
X Ray Diffraction ◽  
X Ray ◽  
Structure And Morphology ◽  
Scanning Electron ◽  
Nm Range

A series of CexZr(1-x)O2 mixed oxides with different ratio (0 x 1) have been synthesized using microemulsion method. The structure and morphology of the mixed oxides have been investigated via X-ray Diffraction (XRD) and Field Emission Scanning Electron Microscopy (FESEM). The results showed that the synthesized mixed oxides were of nanoscale size and the cubic phase was obtained with the application of a ratio of x > 0.5. Additionally, it was found that the tetragonal phase existed with lower ceria content. The average crystallite size of the CexZr(1-x)O2 series were found to be in the 5 - 10 nm range. Moreover, the roughness of these mixed oxides had also decreased with increasing ceria content.

Indium Nitride Nanoparticles Prepared by Laser Ablation in Liquid

2019 ◽  
Vol 18 (02) ◽  
pp. 1850021 ◽  
Author(s):  
Khawla S. Khashan ◽  
Sarah F. Abbas
Keyword(s):  
Electron Microscopy ◽  
Scanning Electron Microscopy ◽  
Fourier Transform ◽  
Laser Ablation ◽  
Indium Nitride ◽  
Fourier Transform Infrared ◽  
Cubic Phase ◽  
X Ray Diffraction ◽  
X Ray ◽  
Scanning Electron

Indium nitride InN nanoparticles NPs suspension prepared by Nd:YAG laser ablation of indium target submerged under ammonium hydroxide. The Scanning electron microscopy, X-ray diffraction, Fourier transform infrared spectroscopy, UV/VIS/NIR spectrophotometer and Conductivity meter were used to determine the properties of the nanoparticles prepared with different laser conditions. Fourier transform infrared spectra exhibit the presence of In[Formula: see text]N and In–N bonds, which indicates the formation of InN particles. X-ray diffraction pattern observed in the formation of InN NPs with cubic phase, the average diameters of the dominant peak c-InN (101) were approximately 2[Formula: see text]nm. Scanning electron microscopy image shows the presence of a large number of spherical shape nanoparticles having a particle size in the range 2–40[Formula: see text]nm with a few individual nanoparticles larger than 128[Formula: see text]nm. The transmission spectra of InN NPs suspension have the maximum optical transmission edge at 1378[Formula: see text]nm with bandgap energy was 0.85–1.2[Formula: see text]eV. InN has high electrical conductivity that depends on temperature value with small activation energy at room temperature ranging from 0.0318[Formula: see text]meV to 0.1591[Formula: see text]meV.

Microstructures in thin BaTiO3 Films by Hydrothermal Method

1997 ◽  
Vol 495 ◽  
Author(s):  
T. Hoffmann ◽  
V. M. Fuenzalida
Keyword(s):  
Electron Microscopy ◽  
Scanning Electron Microscopy ◽  
Barium Titanate ◽  
Hydrothermal Reaction ◽  
Cubic Phase ◽  
X Ray Diffraction ◽  
Titanium Layer ◽  
X Ray ◽  
Lift Off ◽  
Scanning Electron

ABSTRACTBarium titanate microstructures are fabricated on silicon(100)/platinum substrates coated with photoresist and titanium by a combination of hydrothermal and lift-off techniques. The microstructures of 10μm width are well defined. The barium titanate films grow in its cubic phase. Analysis by means of x-ray diffraction and scanning electron microscopy shows that only a part of the titanium layer is affected by the hydrothermal reaction. This limitation may be overcome by application of electrochemistry.

Microraman Spectroscopy and X-Ray Diffraction Studies of Ti-W-O Thin Films

1996 ◽  
Vol 441 ◽  
Author(s):  
Luigi Sangaletti ◽  
Elza Bontempi ◽  
Laura E. Depero ◽  
P. Galinetto ◽  
Silvio Groppelli ◽  
...  
Keyword(s):  
Thin Film ◽  
Electron Microscopy ◽  
Thin Films ◽  
Scanning Electron Microscopy ◽  
Cubic Phase ◽  
X Ray Diffraction ◽  
X Ray ◽  
Different Temperatures ◽  
Microraman Spectroscopy ◽  
Scanning Electron

AbstractThin films of the Ti-W-O system grown by r.f. reactive sputtering from a Ti-W (10%–90% weight) target have been studied by Raman and microraman spectroscopy, X-ray diffraction and scanning electron microscopy with the aim to investigate their microstructural and morphological properties. To this purpose, the kinetics of structural transformations at different temperatures (600 °C, and 800 °C) have been studied, and the effect of Ti on the WO3 lattice has been singled out. The results show that annealing at different temperatures induces a microstructural evolution from the amorphous phase of the as-deposited thin film to WO3 crystalline phases via an intermediate cubic disordered phase of WO3. The effect of Ti on this cubic phase and on the thin film morphology is also investigated with the aid of microraman and scanning electron microscopy analysis. The results show that two distinct phases arise upon long annealing treatments; namely, small crystallites belonging to the WO3 monoclinic phase are dispersed on a layer composed of a disordered cubic WO3 phase with a high Ti content.

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

2020 ◽  
Vol 3 (2) ◽  
pp. 103-113
Author(s):  
Lediliocza Lediliocza ◽  
Sitti Ahmiatri Saptari ◽  
Slamet Priyono
Keyword(s):  
Electron Microscopy ◽  
Scanning Electron Microscopy ◽  
Solid State ◽  
Electrochemical Impedance ◽  
X Ray Diffraction ◽  
Food Grade ◽  
X Ray ◽  
Lithium Titanium ◽  
Charge Discharge ◽  
Scanning Electron

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. 

Identification of calcium oxalate crystals in dried or fixed tobacco leaf

1984 ◽  
Vol 42 ◽  
pp. 288-289
Author(s):  
Vicki L. Baliga ◽  
Mary Ellen Counts
Keyword(s):  
Electron Microscopy ◽  
Scanning Electron Microscopy ◽  
Calcium Oxalate ◽  
Growth And Development ◽  
Polarized Light ◽  
Calcium Oxalate Crystals ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Scanning Electron

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.

Environmental scanning electron microscopy of fresh human gallstones reveals new morphologies of precipitated calcium salts

1992 ◽  
Vol 50 (2) ◽  
pp. 1322-1323
Author(s):  
Howard S. Kaufman ◽  
Keith D. Lillemoe ◽  
John T. Mastovich ◽  
Henry A. Pitt
Keyword(s):  
Electron Microscopy ◽  
Scanning Electron Microscopy ◽  
Environmental Scanning Electron Microscopy ◽  
Environmental Scanning ◽  
X Ray Diffraction ◽  
Calcium Salts ◽  
Cholesterol Gallstones ◽  
X Ray ◽  
Ca Carbonate ◽  
Scanning Electron

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.

PENINGKATAN LAJU DISOLUSI ACYCLOVIR DENGAN METODE SISTEM DISPERSI PADAT MENGGUNAKAN POLOXAMER 188

2016 ◽  
Vol 5 (1) ◽  
pp. 6
Author(s):  
Budi Setiawan ◽  
Erizal Zaini ◽  
Salman Umar
Keyword(s):  
Electron Microscopy ◽  
Thermal Analysis ◽  
Scanning Electron Microscopy ◽  
Fourier Transform ◽  
Differential Thermal Analysis ◽  
Fourier Transform Infrared ◽  
X Ray Diffraction ◽  
Poloxamer 188 ◽  
X Ray ◽  
Scanning Electron

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.

Structural Characterization of Gallbladder Stones Using Energy Dispersive X-ray Spectroscopy and X-ray Diffraction

2018 ◽  
Vol 21 (7) ◽  
pp. 495-500 ◽  
Author(s):  
Hassan A. Almarshad ◽  
Sayed M. Badawy ◽  
Abdalkarem F. Alsharari
Keyword(s):  
Electron Microscopy ◽  
Scanning Electron Microscopy ◽  
Energy Dispersive ◽  
Spectroscopic Techniques ◽  
X Ray Diffraction ◽  
Major Health Problem ◽  
X Ray ◽  
Gallbladder Stones ◽  
Pure Cholesterol ◽  
Scanning Electron

Aim and Objective: Formation of the gallbladder stones is a common disease and a major health problem. The present study aimed to identify the structures of the most common types of gallbladder stones using X-ray spectroscopic techniques, which provide information about the process of stone formation. Material and Method: Phase and elemental compositions of pure cholesterol and mixed gallstones removed from gallbladders of patients were studied using energy-dispersive X-ray spectroscopy combined with scanning electron microscopy analysis and X-ray diffraction. Results: The crystal structures of gallstones which coincide with standard patterns were confirmed by X-ray diffraction. Plate-like cholesterol crystals with laminar shaped and thin layered structures were clearly observed for gallstone of pure cholesterol by scanning electron microscopy; it also revealed different morphologies from mixed cholesterol stones. Elemental analysis of pure cholesterol and mixed gallstones using energy-dispersive X-ray spectroscopy confirmed the different formation processes of the different types of gallstones. Conclusion: The method of fast and reliable X-ray spectroscopic techniques has numerous advantages over the traditional chemical analysis and other analytical techniques. The results also revealed that the X-ray spectroscopy technique is a promising technique that can aid in understanding the pathogenesis of gallstone disease.

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