Study on Hydrothermal Synthesis of Flower-Sphere MoS2

2011 ◽  
Vol 311-313 ◽  
pp. 566-570
Author(s):  
Jun Zhou ◽  
Xin Zhe Lan ◽  
Ping Ren ◽  
Lei Wu

An effective technology of hydrothermal synthesizing flower-sphere MoS2 by reaction of Na2MoO4 and CS(NH2)2 with NH2OH•HCl as reductant was researched. The effect of the molar ratio of Mo to S, reaction temperature, reaction time, aging time on the yield, purity and morphology of the product was explored by means of X-ray diffraction (XRD) and scanning electron microscope (SEM). The results show that the optimal synthesis conditions are as follows: the molar ratio of Mo to S of 1:7, the temperature of 220°C, the reaction time of 24h and the aging time of 16h. Under these conditions, the inerratic and pure flower-sphere MoS2 was obtained. Its average particle size is about 2μm and the petal is self-assembly growth. The yield of the product can reach 88%.

NANO ◽  
2012 ◽  
Vol 07 (04) ◽  
pp. 1250030
Author(s):  
MADJID TORKAMAN ◽  
AZIZAN AZIZ ◽  
MOHAMAD ABU BAKAR ◽  
SULAIMAN AB GHANI

In this work manganese dioxide (Ramsdellite- MnO2 ) was synthesized at room temperature using a facile electrochemical method. X-ray diffraction (XRD) was used to identify the type and the size of the crystal particle, while field emission scanning electron microscopy (FESEM) and energy filtered transmission electron microscopy (EFTEM) were used to show and identify the morphology of the particles and changes of their morphologies with the increase of reaction times. Fourier transform infrared (FTIR) spectroscopy confirmed the Mn–O bond. Results from XRD showed that optimum time for synthesis Ramsdellite- MnO2 was 9 h. The results of EFTEM showed a mixture of nanospheres and nanorods after 9 h reaction time while a homogenous morphology of nanospheres was detected at 12 h reaction time. Results confirmed on the existence of a correlation between the reaction time and the resulting nanostructures. Moreover, the EFTEM result showed that average particle size for 12 h was (25 ± 7 nm). The variation of calculated specific capacitance (F/g) versus the different scan rate has indicated that the efficiency of synthesized Ramsdellite- MnO2 nanostructures in 12 h reaction time was superior to 9 h.


2014 ◽  
Vol 2014 ◽  
pp. 1-10 ◽  
Author(s):  
K. A. Athmaselvi ◽  
C. Kumar ◽  
M. Balasubramanian ◽  
Ishita Roy

This study evaluates the physical properties of freeze dried tropical (guava, sapota, and papaya) fruit powders. Thermal stability and weight loss were evaluated using TGA-DSC and IR, which showed pectin as the main solid constituent. LCR meter measured electrical conductivity, dielectric constant, and dielectric loss factor. Functional groups assessed by FTIR showed presence of chlorides, and O–H and N–H bonds in guava, chloride and C–H bond in papaya, and chlorides, and C=O and C–H bonds in sapota. Particle size and type of starch were evaluated by X-ray diffraction and microstructure through scanning electronic microscopy. A semicrystalline profile and average particle size of the fruit powders were evidenced by X-ray diffraction and lamellar/spherical morphologies by SEM. Presence of A-type starch was observed in all three fruits. Dependence of electric and dielectric properties on frequency and temperature was observed.


2010 ◽  
Vol 177 ◽  
pp. 673-676 ◽  
Author(s):  
Jun Xue ◽  
Hou Kui Xiang ◽  
Hong Qiao Ding ◽  
Shu Li Pang ◽  
Xue Hua Wang ◽  
...  

Carbon encapsulated Fe-Cu alloys nanoparticles were synthesized by using ferric nitrate, copper nitrate as metal sources and using sucrose as carbon source. The synthesis process involved a step of hydrazine hydrate reduction in alcohol solution and a step of annealing carbonization. The as-prepared samples were characterized by X-ray diffraction technique, X-ray energy dispersion spectrograph, trans- mission electron microscopy and Raman spectroscopy. The results showed the sample was core / shell structure, the metalic core was crystalline FeCu4 alloy, the shell was amorphous carbon, and the average particle size was about 51nm. The magnetic measurement by using a vibrating sample magnetometer revealed that the sample has ultra-soft magnetic property with the saturation magnetization Ms of 13.01 emu/g, residual magnetization Mr of 0.37 emu/g and coercive forces Hc of 54.43 Oe at room temperature.


2014 ◽  
Vol 1010-1012 ◽  
pp. 961-965
Author(s):  
Jian Qiang Xiao ◽  
Guo Wei He ◽  
Yan Jin Hu

Bauxite waste sludge as a raw material, the use of reverse chemical coprecipitation synthesize Fe3O4. Researching temperature, precipitation concentration, aging time and Fe2+/Fe3+ molar ratio effect on the particle size, morphology. Optimal experimental conditions: temperature 70 °C, the precipitant NaOH mass ratio of 10%, aging time 3h, Fe2+/Fe3+ molar ratio of 2:3. Test methods using a laser particle size analyzer, XRD analysis of the products were characterized, the product is Fe3O4, the average particle size of 0.11mm.


2020 ◽  
Vol 63 (7) ◽  
pp. 75-78
Author(s):  
Polina A. Bezborodova ◽  
◽  
Elena M. Filonenko ◽  
Kseniya R. Erager ◽  
Anatoly V. Butakov ◽  
...  

Using the data of qualitative X-ray phase analysis, it was shown that in a wide concentration range at 1223 K compounds based on silver niobate are formed in the condition of the heterovalent substitution of tungsten(VI) ions for niobium(V) ions. These compounds are isomorphic to a perovskite-type structure. Microprobe analysis data allows to determine the homogeneity of the analyzed samples and the correspondence of their experimental compositions to the theoretical ones for the formula Ag1-xNb1-xWxO3. Using the data of X-ray diffraction analysis (Rietveld method) in the Crystallography Data Analysis Software – GSAS, the crystal structure of the obtained compounds was refined. The surface morphology of samples having been obtained at 1373 K was investigated by scanning electron microscopy (SEM). It was shown that with an increase of Nb5+ to W6+ substitution degree for Ag1-xNb1-xWxO3 ceramic samples in the range of the (0.2≤x≤0.8) molar ratio, the average particle size for the studied compositions grows from 1.3 to 5.2 μm, respectively. For the obtained ceramic compounds based on silver niobate with a perovskite-like structure (tetragonal distortion), the temperature-frequency dependences of dielectric parameters in the range 300-900 K were studied. It was found that samples slowly cooled from 1373 K are characterized by low values of (ε ~ 10) and loss (tgδ ~ 0.004 at f = 1 kHz) at room temperature. The ceramics obtained are characterized by relatively high values of dielectric permittivity ε at low frequencies and/or high temperatures. The dielectric parameters of the obtained ceramics are similar to the characteristics of so-called "colossal" dielectric constant materials. The revealed features of the dielectric characteristics of quenched ceramics apparently result from Maxwell-Wagner relaxation at intercrystalline contacts.


2013 ◽  
Vol 591 ◽  
pp. 272-276
Author(s):  
Fang Zhang ◽  
Chao Song ◽  
Ling Li Ma ◽  
Xiao Li Xu ◽  
Zi Fei Peng

Sr2CeO4: Ho3+ was prepared by high-temperature solid-state method. The products were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM) and photo luminescent (PL). The Sr2CeO4:Ho3+ phosphors showed a red emission under the near-ultraviolet excitation (280 nm) and the main emission centered at 475 nm. It has been found that A+ (A+ = Li+, Na+ or K+) codoped Sr2CeO4: Ho3+ phosphors could lead to a remarkable increase of photoluminescence. Luminous intensity was the highest when doping Li+ ions. Investigation indicated that Sr2Ce0.989O4: 0.001Ho3+, 0.01Li+ exhibited the strongest emission. The average particle size was about 6 um. The optimum sintering temperature was 1200 °C and the possible mechanism was also discussed.


2014 ◽  
Vol 896 ◽  
pp. 100-103 ◽  
Author(s):  
Anggi Puspita Swardhani ◽  
Ferry Iskandar ◽  
Abdullah Mikrajuddin ◽  
Khairurrijal

Fe2O3/C nanocomposites were successfully synthesized using microwave assisted calcination method. Ferric (III) chloride hexahydrate (FeCl36H2O), sodium hydroxide (NaOH), and dextrose monohydrate (C6H12O6H2O) were used as precursors. A microwave oven of 2.445 GHz with a power of 600 W for 20 minutes was employed during the syntheses. Calcination was performed in a simple furnace at 350 °C for 30 min. The molar ratio of C:Fe is the only process parameter. From Scanning Electron Microscope images, the average particle size were 199 nm and 74 nm for the samples with molar ratio of C:Fe of 1:2 and 1:1, respectively. X-ray diffractometer spectra showed that the obtained samples have γ-Fe2O3 (maghemite) crystal structure. Using the Scherrer method, the crystallite size were 61.7, 58.8, 52.5, and 48.8 nm for the samples with the molar ratios of C:Fe of 1:3, 1:2, 1:1, and 2:1, respectively. It means that the crystallite size of the nanocomposite decreases with the increase of the molar ratio of carbon to iron (C:Fe). The Brunauer-Emmett-Teller characterization showed that the surface area as high as 255.6 m2/g is achieved by of the Fe2O3/C nanocomposite with the molar ratio of C:Fe of 1:1.


2017 ◽  
Vol 9 (2) ◽  
pp. 60 ◽  
Author(s):  
Sudirman Sudirman ◽  
Indriyati Indriyati ◽  
Wisnu Ari Adi ◽  
Rike Yudianti ◽  
Emil Budianto

Synthesis of Pt/CNT composite by using sol gel method has been performed which the composition of CNT on the composite are vary, (x = 20, 40, 60 and 80 wt%). Performance of composite was characterized by Transmission Electron Microscope (TEM) and X-Ray Diffraction (XRD), respectively. In the refinement results of X-ray diffraction pattern, the composite consists of two phases, namely, carbon and platinum phases. Carbon phase has a structure hexagonal (P 63 m c) with lattice parameters a = b = 2.451(2) Å and c = 6.89(1) Å, α = β = 90° and γ = 120°, the unit cell volume of V = 35.8(1) A3, and the atomic density of ρ = 2.224 g.cm-3. While platinum phase has the structure of cubic (F m -3 m) with lattice parameters a = b = c = 3.921(2) Å, α = β = γ = 90°, the unit cell volume of V = 60.3(1) A3, and the atomic density of ρ = 21.487 g.cm-3.According to the image of TEM, the average particle size for Pt nano particle is estimated to range from 4.1-4.3 nm. While the cavity diameter average of CNT is estimated to range from 5.9-7.5 nm. Based on the calculation, the crystallite size of the Pt particle was around 4.31 nm. The optimum value of dispersed Pt into CNT occurred at 60 wt% CNT with the best composition of Pt in the unit cell of cystal structure. We concluded that this study successfully dispersed Pt nanoparticles onto CNT formed Pt/CNT composite. This was a great opportunity that the composite can be applied as electrocatalyst system on fuel cell application.


2012 ◽  
Vol 02 (01) ◽  
pp. 1250007 ◽  
Author(s):  
LAXMAN SINGH ◽  
U. S. RAI ◽  
K. D. MANDAL ◽  
MADHU YASHPAL

Ultrafine powder of CaCu2.80Zn0.20Ti4O12 ceramic was prepared using a novel semi-wet method. DTA/TG analysis of dry powder gives pre-information about formation of final product around 800°C. The formation of single phase was confirmed by X-ray diffraction analysis. The average particle size of sintered powder of the ceramic obtained from XRD and Transmission electron microscopy was found 59 nm and 102 nm, respectively. Energy Dispersive X-ray studies confirm the stoichiometry of the synthesized ceramic. Dielectric constant of the ceramic was found to be 2617 at room temperature at 1 kHz.


2012 ◽  
Vol 554-556 ◽  
pp. 18-22
Author(s):  
Supakorn Silakate ◽  
Anucha Wannagon ◽  
Apinon Nuntiya

The objectives of this study were to prepare leadless crystalline glazes from iron oxide by using low temperature firing (1,100°C) and to study the effect of concentration of iron oxide on the phase composition of the glaze raw materials on phase transformation in leadless iron oxide crystalline glaze. The crystalline phases were investigated by using the DTA, X-ray diffraction (XRD) and scanning electron microscopy (SEM) techniques. The composition of the glaze raw materials compose of nepheline syenite, colemanite, pottery stone, bentonite, ZnO, Li2CO3, SiOSubscript text2 and 10, 15 and 20%(w/w) iron oxide (Fe2O3). The glaze raw materials were ground for homogeneous mixtures by ball milling for 24h. The average particle size of the mixture was 3.86 µm. The glaze bodies were carried to firing at 1,100°C at the heating rate of 2°C/min and soaking for 0.5h. Then, the glaze bodies were cooled at the cooling rate of 1°C/min and maintained at 1,080°C for 3h and then maintained at 980°C for 1h, respectively. From the experiment results, it was found that the crystallization temperatures (Tc) of franklinite (ZnFe2O4) and anorthite (CaAl2Si2O8) depend on the concentration of iron oxide content.


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