Preparation of Nano-spherical Iron Phosphate by Hydrothermal Method and Its Application as the Precursor of Lithium Iron Phosphate

Author(s):  
Ju Guo ◽  
Fuyong Wu

Abstract First, nano-spherical iron phosphate was prepared using the hydrothermal method. Then, the carbothermal reduction method was applied to synthesize the LiFePO4/C composite material capable of good carbon coating effect with the prepared nano-spherical iron phosphate as a precursor. By means of scanning electron microscope, transmission electron microscope, Zeta potentiometer, inductively coupled plasma spectrometer, X-ray diffraction, X-ray photoelectron spectroscopy, electrochemical testing, and other methods, the material was characterized and tested for its morphology, particle size, composition, structure, and electrochemical performance. According to the test results, when the initial mass concentration of Fe3+ in the reaction solution is 2%, the amount of N and S impurity is merely 19 and 27 ppm, respectively. In the meantime, particle size is small, with a range of roughly 50–100 nm, and a spherical morphology is shown. The synthesized LiFePO4/C retains its nano-spherical morphology, which leads to a desirable carbon coating effect and an excellent electrochemical performance. The first charge–discharge specific capacity at 0.1 C rate reached 163.7 and 161.4 mAh/g, the charge–discharge efficiency was 98.6%, and the capacity retention rate at 50 charge–discharge cycles at 1 C rate reached 98.52%.

2018 ◽  
Vol 238 ◽  
pp. 02002
Author(s):  
Fangjing Sun ◽  
Yi Zhang ◽  
Jiawei Zhang ◽  
Xixi Yan ◽  
Xiaoyu Liu ◽  
...  

In this experiment, ultrafine iron phosphate micro-powder was prepared by hydrothermal method which used phosphate slag as an iron source. The effects of reaction temperature, surfactants type and amount on its particle size were explored. The samples were characterized by using Malvern Laser Particle Size Analyzer (MS2000), X-Ray Diffractometer (XRD), Scanning Electron Microscope (SEM) and Energy Dispersive X-Ray Spectroscopy (EDX).The results showed that at 160 °C, 1 wt%CTAB, monoclinic iron phosphate micro-powder was obtained with an average particle size about 0.4 μm which also has a good dispersion in aqueous solution.


2013 ◽  
Vol 860-863 ◽  
pp. 956-959
Author(s):  
Xing Hua Liang ◽  
Lin Shi ◽  
Yu Si Liu ◽  
Tian Jiao Liu ◽  
Chao Chao Ye ◽  
...  

The High Potential Material Lini0.5Mn1.5O4 was Synthesized via Solid-State Reaction.The Surface Morphology and Particle Size of the Sample were Observed by Scanning Electron Microscope(SEM).The Crystal Structure of the Sample was Collected and Analyzed through X-Ray Diffractometry(XRD).The Sample was Charaterized by Charge-Discharge Tests.Results Indicated that the Cycling Retention Rate was about 80%,after being Charge-Diacharged at a Rate of 0.1C in a Voltage of 3.45-4.77V for 10 Times.Compared with Limn2O4,LiNi0.5Mn1.5O4 has good cycle performance.Both of LiNi0.5Mn1.5O4 structure were space group of Fd3m.


2014 ◽  
Vol 1043 ◽  
pp. 7-11
Author(s):  
A.F.M. Fadzil ◽  
F.H. Muhammad

LiMn1.5Fe0.5O4is synthesized using sol-gel method and annealed at 850°C for 24 hours. It is then characterized using X-ray diffraction (XRD) and charge discharge analysis. The bulk material are then proceed to further grinding to become nanosize. The nanosample is then characterized using XRD and charge discharge performance, and the specific capacities of the two materials are compared. nanosample of LiMn1.5Fe0.5O4shows higher specific capacity which is 160.16 mAhg-1compares to the bulk which gives only 128.663mAhg-1. This shows that with smaller particle size, the battery performance has improved in terms of its capacity.


Coatings ◽  
2020 ◽  
Vol 10 (11) ◽  
pp. 1045
Author(s):  
Fuquan Deng ◽  
Hua Jin ◽  
Wei Xu

A series of polydodecylmethylsilsesquioxane (PDMSQ) nanocomposite latexes were prepared via emulsion polymerization of methyltriethoxysilane (MTES) and dodecyltrimethoxysilane (DTMS) and sodium hydroxide as the catalyst, and sodium dodecyl benzene sulfonate/Tween 80 as the mixed emulsifiers. Effects of the emulsifier doses, the reaction temperature, the catalyst concentration and the oil/water ratio on the particle size and distribution of the PDMSQ nanoparticles were discussed. Particle size and micromorphology, structure, thermal stability, crystallinity and hydrophobicity of PDMSQ nanoparticles (PDMSQ NPs) were investigated by dynamic laser scattering (DLS), Fourier transform infrared spectroscopy (FTIR), silicon-nuclear magnetic resonance (28Si-NMR), X-ray photoelectron spectroscope (XPS), scanning electron microscope (SEM), transmission electron microscope (TEM), atomic force microscope (AFM), thermo gravimetric analysis (TGA), X-ray diffraction (XRD) and contact angle tester. Results showed that a series of PDMSQ NPs could be obtained with an average particle size of less than 80 nm and narrow distribution as well as spherical structure under the optimal process conditions. PDMSQ NPs exhibited excellent thermal stability and were mainly amorphous but also contained some crystal structures. Importantly, the static water contact angles (WCAs) on its latex films were larger than 150° and the WCAs hysteresis were less than 10°, thus those PDMSQ nanocomposite latexes show potential in the field of superhydrophobic coatings.


2020 ◽  
Vol 13 (07) ◽  
pp. 2051045
Author(s):  
Kaicheng Yue ◽  
Zhaoqian Yan ◽  
Zhihao Sun ◽  
Anran Li ◽  
Lei Qian

In this work, graphitic carbon nitride (g-C3N4) was modified by Pd nanoparticles (Pd-CN) to prepare an efficient cathode catalyst for Li-O2 batteries. The specific surface area of g-C3N4 was improved to 239.56[Formula: see text]m2/g by two-steps thermal polymerization. Pd nanoparticles were loaded onto the g-C3N4 by K2PdCl4 reduction with NaBH4. The resulted Pd-CN composites were characterized by X-ray diffraction, X-ray photoelectron spectroscopy, field emission scanning electron microscope, and transmission electron microscope. The results proved that g-C3N4 showed three-dimensional layered and porous structure, and Pd nanoparticles were successfully supported on it. The Li-O2 batteries using Pd-CN composites as cathode catalysts were assembled and tested. The maximum initial discharge specific capacity reached 26,614[Formula: see text]mAh[Formula: see text]g[Formula: see text] at current density of 100[Formula: see text]mA[Formula: see text]g[Formula: see text]. The electrodes remained large capacity under high current density, meaning excellent rate capability. Li-O2 batteries containing Pd-CN cathode were continuously cycled for 70 cycles with no loss of capacity and obvious change in the terminal voltage. These electrochemical results indicated that the loading Pd nanoparticles effectively increased specific capacity, reduced overpotential and improved the cyclic stability. The Pd-CN composites are proved to be the promising cathode catalysts for Li-O2 batteries.


2010 ◽  
Vol 177 ◽  
pp. 32-36 ◽  
Author(s):  
An Rong Wang ◽  
Jian Li ◽  
Qing Mei Zhang ◽  
Hua Miao

Weak magnetic ZnFe2O4 nanoparticles were prepared by coprecipitation and treated with different concentrations of Fe(NO3)3 solution. Untreated and treated particles were studied using a vibrating sample magnetometer, transmission electron microscope, by X-ray diffraction, X-ray energy dispersive spectroscopy and X photoelectron spectroscopy. The results showed that, after treatment, the ZnFe2O4/γ-Fe2O3 forms disphase nanoparticles, with enlarged size, enhanced magnetic properties and with a surface parceled with Fe(NO3)3. The size of the particles and their magnetic properties are related to the concentration of the treatment solution. The particle size and magnetic properties could be controlled by controlling the concentration of treating solution, therefore nanoparticles can be more widely used.


2019 ◽  
Vol 9 (19) ◽  
pp. 4032 ◽  
Author(s):  
Luis Zuniga ◽  
Gabriel Gonzalez ◽  
Roberto Orrostieta Chavez ◽  
Jason C. Myers ◽  
Timothy P. Lodge ◽  
...  

We report results on the electrochemical performance of flexible and binder-free α-Fe2O3/TiO2/carbon composite fiber anodes for lithium-ion batteries (LIBs). The composite fibers were produced via centrifugal spinning and subsequent thermal processing. The fibers were prepared from a precursor solution containing PVP/iron (III) acetylacetonate/titanium (IV) butoxide/ethanol/acetic acid followed by oxidation at 200 °C in air and then carbonization at 550 °C under flowing argon. The morphology and structure of the composite fibers were characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), and thermogravimetric analysis (TGA). These ternary composite fiber anodes showed an improved electrochemical performance compared to the pristine TiO2/C and α-Fe2O3/C composite fiber electrodes. The α-Fe2O3/TiO2/C composite fibers also showed a superior cycling performance with a specific capacity of 340 mAh g−1 after 100 cycles at a current density of 100 mA g−1, compared to 61 mAh g−1 and 121 mAh g−1 for TiO2/C and α-Fe2O3/C composite electrodes, respectively. The improved electrochemical performance and the simple processing of these metal oxide/carbon composite fibers make them promising candidates for the next generation and cost-effective flexible binder-free anodes for LIBs.


2010 ◽  
Vol 434-435 ◽  
pp. 850-852
Author(s):  
Qi Wang ◽  
Bo Yin ◽  
Zhen Wang ◽  
Gen Li Shen ◽  
Yun Fa Chen

In present work, ceria microspheres were synthesized by template hydrothermal method. Crystalline form of the as-synthesized ceria microspheres was defined by X-ray powder diffraction (XRD) and high resolution transmission electron microscopy (HRTEM). Dispersibility of ceria microspheres was comprehensively characterized using scanning electron microscope (SEM) observation and laser particle size analyzer. Furthermore, the ultraviolet light absorption performances of ceria microspheres with several different sizes were compared by ultraviolet visible spectrophotometer. The results showed that ceria microspheres presented excellent UV absorbent property and the size influence was remarkable.


2007 ◽  
Vol 121-123 ◽  
pp. 1265-1268 ◽  
Author(s):  
T.A. Han ◽  
J.P. Tu ◽  
Jian Bo Wu ◽  
Y.F. Yuan ◽  
Y. Li

Al-substituted α-Ni(OH)2 was synthesized by a chemical co-precipitation. The as-prepared α-Ni(OH)2 particles were characterized by the means of X-ray diffraction (XRD) and scanning electron microscope (SEM). The obtained α-Ni(OH)2 particles were well crystallized, spherical shape with the particle sizes of 20-35 nm. The electrochemical performance of β-Ni(OH)2 electrode with addition of nanosized α-Ni(OH)2 was investigated by galvanostatic charge-discharge tests. The nanosized α-Ni(OH)2 as additive in the commercial microsized spherical β-Ni(OH)2 electrode improved the discharge capability. As compared to commercial β-Ni(OH)2 electrode, the electrode with nanosized α-Ni(OH)2 exhibited excellent better charge-discharge cycling stability. It may be a promising positive active material for alkaline secondary batteries.


2011 ◽  
Vol 04 (04) ◽  
pp. 319-322 ◽  
Author(s):  
AI FANG LIU ◽  
ZU BIAO WEN ◽  
YA FEI LIU ◽  
ZHONG HUA HU

LiFe 1-x Mn x PO 4/ C composites were prepared as cathode material for lithium ion battery via solid-state reaction and using glucose as reducing agent and carbon source. The crystal structure and morphology were investigated by X-ray diffraction (XRD), scanning electron microscope (SEM) and transmission electron microscope (TEM). The resultant samples were pure olivine compounds with an orthorhombic structure. Their electrochemical performance was studied by galvanostatic charge–discharge test and cyclic voltammetry. The results showed that the sample LiFe0.8Mn0.2PO4/C with an average particle size of 400 nm exhibited the largest discharge capacity of 150 mAh g-1, excellent reversibility of charge–discharge and high capacity retention of 97% after a 50-cycle CV scanning. The improved electrical conductivity corresponding to the fine carbon layer around the LiFe0.8Mn0.2PO4 individual particle can be responsible for all these excellent electrochemical performance.


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