Metallothermic Reduction at Low Temperature Synthesis of Ti4O7 Powder with Lithium Ion Insertion/Extraction Property

2019 ◽  
Vol 956 ◽  
pp. 55-66
Author(s):  
Bei Lei Yan ◽  
Wei Wei Meng ◽  
San Chao Zhao

In this work, a thermal reduction process via ultrafine titanium powder as the reducing agent under argon atmosphere is firstly used to prepare Ti4O7. Compared with the conventional method, this experiment process reduces the sintering temperature to 850°C. The phase transformation and the morphology of the as-prepared powders are examined by X-Ray diffraction (XRD) and scanning electron microscopy (SEM). Besides, it is found that the Ti4O7 powders obtained by titanium thermal reduction method exhibited the crystal structure, distinctly possessing an average particle size around 750 nm. The as-prepared Ti4O7 nanoparticles are used as anode active material in lithium battery. The results demonstrate that the anode with Ti4O7 calcined at 850°C by titanium thermal reduction method exhibited insertion/extraction lithium ion property.

2017 ◽  
Author(s):  
Yusnita Rifai

AbstrakNanopartikel perak telah disintesis menggunakan metode reduksi. Dalam penelitian ini, ekstrak metanol daun Kemangi (Ocimum citriodorum) digunakan sebagai agen pereduksi untuk prekursor AgNO3. Sintesis nanopartikel perak dilakukan dengan mencampurkan laru- tan AgNO3 1mM dengan filtrat ekstrak daun kemangi. Hasil karakterisasi UV-Vis menun- jukkan bahwa nilai absorbansi meningkat dengan meningkatnya waktu kontak reaksi. Pun- cak absorbansi spektrum UV-Vis dari sampel biosintesis nanopartikel perak berkisar pada 427-439 nm selama 1 hari dengan pengadukan dan penyimpanan. Ukuran nanopartikel perak ditentukan menggunakan Pengukur Ukuran Partikel (PSA) dengan rata-rata distribusi uku- ran partikel sebesar 57,38 nm. Efek mekanik dalam proses biosintesis nanopartikel perak cenderung mempercepat pembentukan nanopartikel perak. Hasil karakterisasi menggunakan Difraksi Sinar-X (XRD) diketahui kristalit yang terbentuk memiliki intensitas terbesar pada sudut 38° dengan nilai FWHM 0,66310 (ukuran 0,3 nm) dalam sistem kristal kubik.Kata kunci: Biosintesis, Nanopartikel Perak, Ocimum citriodorum, Karakterisasi AbstractSynthesis of silver nanoparticles by using the reduction method with methanol extract basil (Ocimum citriodorum) leaves, which acted as a reducing agent for AgNO3 precursor have been conducted. Synthesis nanoparticles was carried out by mixing the solution of AgNO3 1mM with filtrate extract of Ocimum leaves. The results of characterization showed that absorbance values increased with the increase in reaction time. Peak of UV-Vis absorption spectrum of biosynthesis sample of silver nanoparticles with stirring and storage each at a wavelength 427-439 nm for 1 day. Silver nanoparticles size was determined by using PSA (Particles Size Analyzer) with an average particle size distribution of 57,38 nm. Mechanical effect in biosynthesis process of silver nanoparticles tends to speed up the formation of silver nanoparticles. The result of characterization by using X-Ray Diffraction (XRD) described that the formed crystal had the angle of 38° with the value of FWHM 0,66310 (sixe 0.3 nm) in cubic crystal system.Key word: Biosynthesis, Silver Nanoparticles, Ocimum citriodorum, Characterization.


2010 ◽  
Vol 17 (02) ◽  
pp. 223-228
Author(s):  
JAE-SIK YOON

Niobium powder was fabricated by metallothermic reduction process using K2NbF7 as the raw material, KCl and KF as the diluents and Na as the reducing agent. The apparatus for the experiment was designed and built specifically for the present study. Varying properties of niobium powder depending on reaction temperature and excess of reducing agent were analyzed. The niobium particle size increased significantly as the reduction temperature increased from 993 to 1093 K. The particle size was fairly uniform at a given reaction temperature, varying from 0.2 μ m to 50 nm depending on the reaction temperature. The yield of niobium powder increased from 58 to 83% with an increase in reaction temperature. The average particle size of niobium powder was improved from 70 nm to 0.2 μ m with the increase in the amount of Na excess. In addition, the yield rate of Nb powder was 82% in the 5% excess sodium.


Author(s):  
Pratik Kumar Jagtap ◽  
Rupesh Kumar Meher ◽  
Madhuri Madhusmita Biswal

Background: The synthesis of metal Nanoparticles is a growing area of research interest due to its potential in the applications and development of advanced technologies. Here we have stressed on the Facile green synthesis approach that connects the nanotechnology and biotechnology. Methods: The method involves use of biological reducing agent cum stabilizing agent (capping agent). A comparative account of particle dimension and surface properties of the synthesized nano particles using Broccoli (Brassicaoleracea var.italica) extract is also presented. Results: The reduction process used in the synthesis was simple and convenient to handle and monitored by UV--Vis spectroscopy showing the absorbance maxima of various samples at 322nm, 496nm and 536nm using different solvents. The presence of active proteins and phenolic groups present in biomass before and after reduction was identified by FTIR. Conclusion: The crystalline morphology and size of the Nanoparticles were examined by TEM, SEM and X-ray diffraction studies, which showed the average particle size of Silver Nanoparticles in the range of 40- 50 nm as well as revealed their FCC structure.


2014 ◽  
Vol 1643 ◽  
Author(s):  
Rob Cook ◽  
Matthew Schrandt ◽  
Praveen Kolla ◽  
Wendell Rhine ◽  
Ranjit Koodali ◽  
...  

ABSTRACTThree types of silica materials with different morphology, specifically SiO2 hollow microspheres, mesoporous silica, and silica aerogel were tested as potential precursors for synthesis of silicon nano- and meso-structures that resemble the original morphology of the precursors. In the optimized magnesium thermal reduction process, magnesium vapor was delivered to silica surface through a stainless steel mesh placed on top of a zirconia boat filled with silica precursor. This approach allowed for better control of silicon nanostructure formation by minimizing reaction by-products that can affect performance of lithium ion battery anode. Material morphological properties of the reduced silica precursors are discussed in terms of X-ray diffraction, BET, BJH pore size distribution, Raman spectroscopy, and TGA.


2007 ◽  
Vol 124-126 ◽  
pp. 1225-1228 ◽  
Author(s):  
Dong Won Lee ◽  
Ji Hun Yu ◽  
Tae Suk Jang

Nanoparticles of TiC and TiCN were synthesized by a magnesium thermal reduction process. The process was performed in the sequence of (1) the transfer of TiCl4+C2Cl4 solutions into a liquefied magnesium protected with Ar, (2) the magnesium reduction of metal chlorides, (3) the formation of a titanium carbide by the reaction of Ti and C atoms released by the magnesium reduction, and finally (4) the vacuum separation of the residual liquid Mg and MgCl2. Titanium carbonitride could be synthesized by maintaining the reaction chamber in nitrogen atmosphere. The average particle size of both TiC and TiCN synthesized was about 80 nm each. The composition of the TiC nanoparticles was approximately TiC0.95 with 0.9 wt % free carbon whereas that of the TiCN nanoparticles was TiC0.46~0.53N0.46~0.51 with 0.1 wt % free carbon.


Nanomaterials ◽  
2021 ◽  
Vol 11 (5) ◽  
pp. 1097
Author(s):  
Luran Zhang ◽  
Xinchen Du ◽  
Hongjie Lu ◽  
Dandan Gao ◽  
Huan Liu ◽  
...  

L10 ordered FePt and FePtCu nanoparticles (NPs) with a good dispersion were successfully fabricated by a simple, green, one-step solid-phase reduction method. Fe (acac)3, Pt (acac)2, and CuO as the precursors were dispersed in NaCl and annealed at different temperatures with an H2-containing atmosphere. As the annealing temperature increased, the chemical order parameter (S), average particle size (D), coercivity (Hc), and saturation magnetization (Ms) of FePt and FePtCu NPs increased and the size distribution range of the particles became wider. The ordered degree, D, Hc, and Ms of FePt NPs were greatly improved by adding 5% Cu. The highest S, D, Hc, and Ms were obtained when FePtCu NPs annealed at 750 °C, which were 0.91, 4.87 nm, 12,200 Oe, and 23.38 emu/g, respectively. The structure and magnetic properties of FePt and FePtCu NPs at different annealing temperatures were investigated and the formation mechanism of FePt and FePtCu NPs were discussed in detail.


Materials ◽  
2021 ◽  
Vol 14 (12) ◽  
pp. 3193
Author(s):  
Tu Lan ◽  
Xiaolong Guo ◽  
De Li ◽  
Yong Chen

The memory effect of lithium-ion batteries (LIBs) was first discovered in LiFePO4, but its origin and dependence are still not clear, which is essential for regulating the memory effect. In this paper, a home-made spray drying device was used to successfully synthesize LiFePO4 with an average particle size of about 1 μm, and we studied the influence of spray drying temperature on the memory effect of LiFePO4 in LIBs. The results showed that the increasing of spray drying temperature made the memory effect of LiFePO4 strengthen from 1.3 mV to 2.9 mV, while the capacity decreased by approximately 6%. The XRD refinement and FTIR spectra indicate that the enhancement of memory effect can be attributed to the increment of Li–Fe dislocations. This work reveals the dependence of memory effect of LiFePO4 on spray drying temperature, which will guide us to optimize the preparation process of electrode materials and improve the management system of LIBs.


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.


2014 ◽  
Vol 2014 ◽  
pp. 1-4 ◽  
Author(s):  
K. R. Nemade ◽  
S. A. Waghuley

Solvent mixed spray pyrolysis technique has attracted a global interest in the synthesis of nanomaterials since reactions can be run in liquid state without further heating. Magnesium oxide (MgO) is a category of the practical semiconductor metal oxides, which is extensively used as catalyst and optical material. In the present study, MgO nanoparticles were successfully synthesized using a solvent mixed spray pyrolysis. The X-ray diffraction pattern confirmed the formation of MgO phase with an excellent crystalline structure. Debye-Scherrer equation is used for the determination of particle size, which was found to be 9.2 nm. Tunneling electron microscope analysis indicated that the as-synthesized particles are nanoparticles with an average particle size of 9 nm. Meanwhile, the ultraviolet-visible spectroscopy of the resulting product was evaluated to study its optical property via measurement of the band gap energy value.


1997 ◽  
Vol 496 ◽  
Author(s):  
David J. Derwin ◽  
Kim Kinoshita ◽  
Tri D. Tran ◽  
Peter Zaleski

AbstractSeveral types of carbonaceous materials from Superior Graphite Co. were investigated for lithium ion intercalation. These commercially available cokes, graphitized cokes and graphites have a wide range of physical and chemical properties. The coke materials were investigated in propylene carbonate based electrolytes and the graphitic materials were studied in ethylene carbonate / dimethyl solutions to prevent exfoliation. The reversible capacities of disordered cokes are below 230 mAh / g and those for many highly ordered synthetic (artificial) and natural graphites approached 372 mAh / g (LiC6). The irreversible capacity losses vary between 15 to as much as 200 % of reversible capacities for various types of carbon. Heat treated cokes with the average particle size of 10 microns showed marked improvements in reversible capacity for lithium intercalation. The electrochemical characteristics are correlated with data obtained from scanning electron microscopy (SEM), high resolution transmission electron microscopy (TAM), X - ray diffraction (XRD) and BET surface area analysis. The electrochemical performance, availability, cost and manufacturability of these commercial carbons will be discussed.


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