Synthesis and electrochemical properties of Cr-doped Li<Subscript>3</Subscript>V<Subscript>2</Subscript>(PO<Subscript>4</Subscript>)<Subscript>3</Subscript> cathode materials for lithium-ion batteries

Cr-doped Li₃V₂(PO₄)₃ cathode materials Li₃V_2−x Cr _x (PO₄)₃ were prepared by a carbothermal reduction(CTR) process. The properties of the Cr-doped Li₃V₂(PO₄)₃ were investigated by X-ray diffraction (XRD), scanning electron microscopic (SEM), and electrochemical measurements. Results show that the Cr-doped Li₃V₂(PO₄)₃ has the same monoclinic structure as the undoped Li₃V₂(PO₄)₃, and the particle size of Cr-doped Li₃V₂(PO₄)₃ is smaller than that of the undoped Li₃V₂(PO₄)₃ and the smallest particle size is only about 1 μm. The Cr-doped Li₃V₂(PO₄)₃ samples were investigated on the Li extraction/insertion performances through charge/discharge, cyclic voltammogram (CV), and electrochemical impedance spectra(EIS). The optimal doping content of Cr was that x=0.04 in the Li₃V_2−x Cr _x (PO₄)₃ samples to achieve high discharge capacity and good cyclic stability. The electrode reaction reversibility was enhanced, and the charge transfer resistance was decreased through the Cr-doping. The improved electrochemical performances of the Cr-doped Li₃V₂(PO₄)₃ cathode materials are attributed to the addition of Cr³⁺ ion by stabilizing the monoclinic structure. Funded by the Guangxi Natural Science Foundation(No. 0832259) and the National Basic Research Program of China (No. 2007CB613607)     

Synthesis and electrochemical properties of Mg-doped LiNi<Subscript>0.6</Subscript>Co<Subscript>0.2</Subscript>Mn<Subscript>0.2</Subscript>O<Subscript>2</Subscript> cathode materials for Li-ion battery

The layered LiNi0.6Co0.2-xMn0.2MgxO2 (x=0.00,0.03,0.05,0.07) cathode materials were prepared by a co-precipitation method.The properties of the Mg-doped LiNi0.6Co0.2Mn0.2O2 were investigated by X-ray diffraction (XRD),scanning electron microscopy (SEM),and electrochemical measurements.XRD studies showed that the Mg-doped LiNi0.6Co0.2Mn0.2O2 had the same layered structure as the undoped LiNi0.6Co0.2Mn0.2O2.The SEM images exhibited that the particle size of Mg-doped LiNi0.6Co0.2Mn0.2O2 was finer than that of ...     

Synthesis and performance of LiMnO<Subscript>2</Subscript> as cathodes for Li-ion batteries

Two structure types of LiMnO₂ were synthesized by sol-gel method and ion-exchange method respectively. The results indicate that orthorhombic phase LiMnO₂ is more stable than layered LiMnO₂, o-LiMnO₂ can be synthesized directly by sol-gel methods followed by heat-treated in argon, but layered LiMnO₂ was obtained only by indirect methods such as ion-exchange method. In this paper, we first synthesized layered NaMnO₂ by the sol-gel method, and then obtained layered LiMnO₂ by the ion-exchange method. The phase, constitution, chemical composition, and images of the products were tested by XRD, AAS (atomic absorption spectroscopy) and SEM. The electrochemical performances of the two structural types of LiMnO₂ are obviously different during the initial few cycles, but later they both have a good capacity-retaining ability. The capacity of layered structure LiMnO₂ is higher than that of o-LiMnO₂. ZHAO Shi-xi: Born in 1966 Funded by the National Natural Science Foundation of China (No.59972026)     

Preparation and electrochemical performance of spherical Fe<Subscript>3</Subscript>O<Subscript>4</Subscript> as anode materials for Li-ion batteries

Fe₃O₄ nano-powder was prepared by the hydrothermal method. The structure and morphology of the product were characterized by X-ray diffraction (XRD) and scanning electronic microscopy (SEM). The as-prepared powder has regularly spherical morphology, and the average size of product is about 25 nm. The possible application use of this material as the active mass of anode for rechargeable Li batteries was examined by cyclic voltammeter (CV), galvanostatic charge/discharge. The experimental results showed that this material exhibited large specific capacity at the first cycle, and the discharge and charge capacity retention of this electrode are 37.04% and 48.76%, respectively. Furthermore, the impedance change of Fe₃O₄ electrode under different cycle number and potential was examined.     

Preparation and electrochemical studies of Y-doped LiVPO<Subscript>4</Subscript>F cathode materials for lithium-ion batteries

Y-doped LiVPO₄F cathode materials were prepared by a carbothermal reduction(CTR) process. The properties of the Y-doped LiVPO₄F samples were investigated by X-ray diffraction (XRD) and electrochemical measurements. XRD studies show that the Y-doped LiVPO₄F samples have the same triclinic structure as the undoped LiVPO₄F. The Li extraction/insertion performances of Y-doped LiVPO₄F samples were investigated through charge/discharge, cyclic voltammogram (CV), and electrochemical impedance spectra(EIS). The optimal doping content of Y is x=0.04 in LiY _x V_1−x PO₄F system. The Y-doped LiVPO₄F samples show a better cyclic ability. The electrode reaction reversibility is enhanced, and the charge transfer resistance is decreased through the Y-doping. The improved electrochemical performances of the Y-doped LiVPO₄F cathode materials are attributed to the addition of Y³⁺ ion by stabilizing the triclinic structure. Funded by the Sponsor Teams for Innovation in the Construction of Talent Highlands in Guangxi Institutions of Higher Learning(GuiJiaoRen [2007]71), Guangxi Natural Science Foundation(No.0832259), the Research Funds of the Guangxi Key Laboratory of Environmental Engineering, Protection and Assessment Program to Sponsor Teams for Innovation in the Construction of Talent Highlands in Guangxi Institutions of Higher Learning(GuiJiaoRen [2007]71)     

Thermal stability of LiFePO<Subscript>4</Subscript>/C-LiMn<Subscript>2</Subscript>O<Subscript>4</Subscript> blended cathode materials

Safety is important to lithium ion battery materials. The thermal stability of LiFePO₄/C-LiMn₂O₄ blended cathode materials is characterized by using TG, XRD, and SEM etc. The results show that LiFePO₄/C-LiMn₂O₄ possesses a worse thermal stability than pure spinel LiMn₂O₄ and pure olivine LiFePO₄/C. When LiFePO₄/C-LiMn₂O₄ blended cathode materials are sintered at 500°C under Ar atmosphere, the sintered cathode materials emit O₂, and appear impurity phases (Li₃PO₄, Fe₂O₃, Mn₃O₄). It is deduced that some chemical reactions take place between different materials, which leads to a worse discharge specific capacity. LiFePO₄/C-LiMn₂O₄ blended cathode materials, therefore, need to be managed and controlled strictly for the sake of thermal stability and safety.     

Direct synthesis of Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-modified Li(Ni<Subscript>0.5</Subscript>Co<Subscript>0.2</Subscript>Mn<Subscript>0.3</Subscript>)O<Subscript>2</Subscript> cathode materials for lithium ion batteries

To improve the cyclic stability at high temperature and thermal stability, the spherical Al₂O₃-modified Li(Ni_0.5Co_0.2Mn_0.3)O₂ was synthesized by a modified co-precipitation method, and the physical and electrochemical properties were studied. The TEM images showed that Li(Ni_0.5Co_0.2Mn_0.3)O₂ was modified successfully with nano-Al₂O₃. The discharge capacity retention of Al₂O₃-modified Li(Ni_0.5Co_0.2Mn_0.3)O₂ maintained about 99% after 200 cycles at high temperature (55 °C), while that of the bare one was only 86%. Also, unlike bare Li(Ni_0.5Co_0.2Mn_0.3)O₂, the Al₂O₃-modified material cathode exhibited good thermal stability.     

Electrochemical Characterization of Surface-modified LiMn2O4 Cathode Materials for Li-ion Batteries

To improve the performance, the surface of 12Mn2O4 was coated with very fine MgO , Al2O3 and ZnO by solgel method, respectively. The structure and morphology of the coated materials were investigated by X-ray diffraction （ XRD ）, X-ray photoelectron spectroscopy （ XPS ） and scanning electron microscopy （SEM）. The charge and discharge performance of uncoated and surfnce modified 12Mn2O4 spinel at 25℃ and 55 ℃ were tested, using a voltage window of 3.0-4.35 V and a current deasity of 0. 1 C rate. There is a slight decrease in the initial discharge capacity relative to that of uncoated UMn2 O4, bat the cycle ability of 12 12Mn2O4 coated by metal-oxide has remarkably been improved. The EIS measuremeuts of uncoated and Al2O3 -coated 12Mn2O4 were carried out by a model 273 A potentiostatl galvanistat controUed by a computer using M270 software, and using a freqnency response analyzer （ Zsimpwin ） combined with a potentiostate （ PAR 273）. Coaseqnently, the reason for the improved cycle properties is that the surface modification reduces the dissolution of Mn , which results from the suppression of the electrolyte decomposition, and suppresses the formation of passivation film that acts as an electronic insulating layer. In conclusion, the use of surface modification is an effective way to improve the electrochemical performance of 12Mn2O4 cathode material for lithium batteries.     

Controllable preparation and superior rate performance of spinel LiMn<Subscript>2</Subscript>O<Subscript>4</Subscript> hollow microspheres as cathode material for lithium-ion batteries

Spinel LiMn₂O₄ microspheres and hollow microspheres with adjustable wall thickness have been prepared using controllable oxidation of MnCO₃ microspheres precursors and following solid reactions with lithium salts. Scanning electron microscopy (SEM) investigations demonstrate that the microsphere morphology and hollow structure of precursors are inherited. The effect of hollow structure properties of as-prepared LiMn₂O₄ on their performance as cathode materials for lithium-ion batteries has been studied. Electrochemical performance tests show that LiMn₂O₄ hollow microspheres with small wall thickness exhibit both superior rate capability and better cycle performance than LiMn₂O₄ solid microspheres and LiMn₂O₄ hollow microspheres with thick wall. The LiMn₂O₄ hollow microspheres with thin wall have discharge capacity of 132.7 mA·h·g^-1 at C/10 (14.8 mA·g^-1) in the first cycle, 94.1% capacity retention at C/10 after 40 cycles and discharge capacity of 116.5 mAh·g^-1 at a high rate of 5C. The apparent lithium-ion diffusion coefficient (D _app) of as-prepared LiMn₂O₄ determined by capacity intermittent titration technique (CITT) varies from 10^-11 to 10^-8.5 cm²·s^-1 showing a regular “W” shape curve plotted with test voltages. The Dapp of LiMn₂O₄ hollow microspheres with thin wall has the largest value among all the prepared samples. Both the superior rate capability and cycle stability of LiMn₂O₄ hollow microspheres with thin wall can be ascribed to the facile ion diffusion in the hollow structures and the robust of hollow structures during repeated cycling.     

Effect of temperature on polishing and flatting time of float-formed Li<Subscript>2</Subscript>O-Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-SiO<Subscript>2</Subscript> glass

Li₂O-Al₂O₃-SiO₂ glass prepared from traditional melting and cooling process was investigated. The surface characteristic of LAS glass was studied by simulating tin bath with different temperature and time, and the effect of surface tension/viscosity ratio on flatting time was analyzed. The results demonstrated that LAS glass can polish effectively when polishing at 1 300 for 8 °C min, and the optimum flatting and polishing temperature was 1 250–1 300 °C.     

低成本动力锂离子电池磷酸铁锂正极材料的合成及性能

磷酸铁锂作为动力锂离子电池的正极材料的首选,正逐渐走向市场.以廉价的Li₃PO₄,FePO₄,Fe粉为原料,一步合成了LiFePO₄/C正极材料,系统研究了葡萄糖、蔗糖和柠檬酸三种不同的碳源对磷酸铁锂性能的影响.采用TG-DTA,XRD,SEM,TEM等手段对产物进行了表征,并研究了其电化学性能.实验结果表明,以葡萄糖为碳源的LiFePO₄/C性能最好,样品颗粒呈球形,表面光滑,分散性好,颗粒表面包覆有2 nm厚的石墨碳层,颗粒之间有碳纤维连接.该样品在0.1 C充放电时首周放电容量达到162.1 mAh/g,20周之后仍然保持在155 mAh/g,显示出良好的循环性能.     

Synthesis and Characterization of LiCoxMn2-xO4 Cathode Materials

LiCoxMn2.04 cathode materials for lithium ion batteries were synthesized by mechanical activation-solid state reaction at 750 ℃ for 24 h in air atmosphere, and their crystal structure, morphology, element composition and electrochemical performance were characterized with XRD, SEM, ICP-AES and charge-discharge test. The experimental results show that all samples have a single spinel structure, well formed crystal shape and uniformly particle size distribution. The lattice parameters of LiCo Mn2-xO4 decrease and the average oxidation states of manganese ions increase with an increase in Co content. Compared with pure LiMn2O4, the LiCo Mn2xO4 （x=0.03-0.12） samples show a lower special capacity, but their cycling life are improved. The capacity loss of LiCo009Mn191O4 and LiCo0.1Mn1.88O4 is only 1.85% and 0.95%, respectively, after the 20th cycle. The improvement of the cycle performance is attributed to the substitution of Co at the Mn sites in the spinel structure, which suppresses the Jahn-Teller distortion and improves the structural stability.     

Synthesis and characterization of ultra-fine Cr<Subscript>2</Subscript>O<Subscript>3</Subscript> from hydrogen reduction of K<Subscript>2</Subscript>CrO<Subscript>4</Subscript>

As a part of the green process for manufacturing chromium compounds, two steps are involved in the synthesis of ultra-fine Cr2O3 powders： the first is the hydrogen reduction of K2CrO4 into intermediate trivalent （Cr^3＋） or tetravalent （Cr^4＋） chromium compounds; the second is the decomposing of the intermediate into Cr2O3 by heat treating. The intermediate is well characterized by means of SEM, XRD, and XPS. The possible reaction mechanism of the process is analyzed.     

Synthesis of polyaniline-Fe<Subscript>3</Subscript>O<Subscript>4</Subscript> nanocomposites and their conductivity and magnetic properties

By using inorganic Fe₃O₄ nanoparticles of different content as nucleation sites, PAn-Fe₃O₄ nanorods were successfully synthesized through a simple, conventional, and inexpensive one-step in-situ polymerization method. The TEM images revealed the size and morphology of the resultant nanocomposite. The EDS pattern confirmed the existence of Fe₃O₄ in the composite. The FT-IR spectral analysis confirmed the formation of PAn encapsulated Fe₃O₄ nanocomposite. With the content of Fe₃O₄ increasing, the conductivity of the nanocomposites gradually decreases, meanwhile, the saturation magnetization increases and reveals a super paramagnetic behavior. With controllable electrical, magnetic, and electromagnetic properties, the well-prepared nanocomposites may have the potential applications in chemical sensors, catalysis, microwave absorbing, and electro-magneto-rheological fluids, etc.     

Preparation and piezoelectric properties of CuO-added (Ag<Subscript>0.75</Subscript>Li<Subscript>0.1</Subscript>Na<Subscript>0.1</Subscript>K<Subscript>0.05</Subscript>)NbO<Subscript>3</Subscript> lead-free ceramics

CuO-doped (Ag_0.75Li_0.1Na_0.1K_0.05)NbO₃ (ALNKN-xCuO, x = 0–2mol%) lead-free piezoelectric ceramics were prepared by the solid-state reaction method in air atmosphere. The effects of CuO addition on the phase structure, microstructure, and piezoelectric properties of the ceramics were investigated. The experimental results show that the ALNKN ceramics without doping CuO possess rhombohedral phase along with K2Nb6O16-type phase and metallic silver phase. For all of the CuO-doped ALNKN ceramics, a pure perovskite structure with the orthorhombic phase was obtained by enclosing the samples in a corundum tube. A homogeneous microstructure with the grain size of about 1 μm was formed for the ceramics with 0.5mol% CuO. The grain size increases with increasing amount of CuO. The temperature dependence of dielectric properties indicates that the ferroelectric phase of the ALNKN-xCuO ceramics becomes less stable with the addition of CuO. The ceramics with x = 1mol% exhibit relatively good electrical properties along with a high Curie temperature. These results will provide a helpful guidance to preparing other AN-based ceramics by solid-state reaction method in air atmosphere.     

Preparation and characterization of nanocomposite MgFe<Subscript>2</Subscript>O<Subscript>4</Subscript>/SiO<Subscript>2</Subscript>

Nanocomposites MgFe₂O₄/SiO₂ were successfully synthesized by the sol-gel method in the presence of N, N-dimethylformamide (DMF). The formation of pure MgFe₂O₄ was confirmed by powder X-ray diffraction (XRD) and electron diffraction. The structural evolution of MgFe₂O₄ nanocrystals was followed by powder X-ray diffraction and IR absorption spectroscopy. The formation of spinel structure of MgFe₂O₄ started at 800 °C, and completed at 900 °C. The transmission electron microscopy (TEM) measurements suggest that the particle sizes increase with the increasing annealing temperature, and the mean particle sizes of the spherical samples annealed at 800 °C, 900 °C and 1 050 °C are ca. 3 nm, 8 nm and 11 nm, respectively. Magnetization measurements at room temperature and 78 K indicate superparamagnetic nature of these MgFe₂O₄ nanocrystals. Funded by the National Natural Science Foundation of China(No. 30771676), the Natural Science Foundation of Jiangsu Province (No. BK20081842), and the Foundation of Nanjing Bureau of Personal for the Returned Overseas Chinese Excellent Scholars     

Microstrueturc and Mcehanieal Propcrtics of Heat-treated GeSb2Te4 Thin Films

The effect of annealing on microstructure, adhesive and frictional properties of GeSb2Te4 films were experimentally studied. The GeSb2Te4 films were prepared by radio frequency （RF） magnetron sputtering, and annealed at 200℃ and 340℃ under vacuum circumstance, respectively. The adhesion and friction experiments were mainly conducted with a lateral force microscope （LFM） for the GeSb2Te4 thin films before and after annealing. Their morphology and phase structure were analyzed by using atomic force microscopy （AFM） and X-ray Diffraction （XRD） techniques, and the nanoindention was employed to evaluate their hardness values. Moreover, an electric force microscope （EFM） was used to measure the surface potential. It is found that the deposited GeSb2Te4 thin film undergoes an amorphous-to-fcc and fcc-to-hex structure transition; the adhesion has a weaker dependence on the surface roughness, but a certain correlation with the surface potential of GeSb2Te4 thin films. And the friction behavior of GeSb2Te4 thin films follows their adhesion behavior under a lower applied load. However, such a relation is replaced by the mechanical behavior when the load is relatively higher. Moreover, the GeSb2Te4 thin film annealed at 340℃ presents a lubricative property.     

Structure and properties of Mg-doped SrBi<Subscript>4</Subscript>Ti<Subscript>4</Subscript>O<Subscript>15</Subscript> Bi-layered compounds

The structure and properties of Mg-doped SrBi4Ti4O15（SBT） were dicussed. Mg substitution into SBT had two possibilities states with the dopant amount variety. Mg cation substituted mostly into Sr^2＋ and the amount proportion was 68.11%.Mg ion will substitute into Ti ion site in perovskite layer when the doping amount increases. Polarization increases sharply when x=0.1 and then decreases becauses of the domain pinning. The Curie temperature of Mg-doped SBT is about 300 ℃ and there is a broad diffuse phase transition near Tc with a flat peak near the Ta of SBT.     

Low-temperature sintering and microwave dielectric properties of Ba<Subscript>2</Subscript>Ti<Subscript>3</Subscript>Nb<Subscript>4</Subscript>O<Subscript>18</Subscript> ceramics

The effects of CuO and H3BO3 additions on the low-temperature sintering,microstructure,and microwave dielectric properties of Ba2Ti3Nb4O18 ceramics were investigated.The addition of less amount of CuO (< 1 wt%) considerably facilitated the densification of Ba2Ti3Nb4O18 ceramics.Appropriate addition of H3BO3 (< 3.5 wt%) remarkably improved the microwave dielectric properties of ceramics.The addition of H3BO3 and CuO successfully reduced the sintering temperature of Ba2Ti3Nb4O18 ceramics from 1300 to 1050 ℃.B...     

Optical and magnetic properties of Fe<Subscript>2</Subscript>O<Subscript>3</Subscript>/SiO<Subscript>2</Subscript> nano-composite films

Fe₂O₃/SiO₂ nano-composite films were prepared by sol-gel technique combining heat treatment in the range of 100–900 °C. The particle size was observed by FE-SEM. Optical properties of the films were investigated by UV-visible spectra. Structural and magnetic characteristics were investigated through FT-IR and VSM. The transparency of the Fe₂O₃/SiO₂ nano-composite films decreased with the content of the Fe₂O₃. Water and organic solvent in the films were evaporated with heat treatment, so the transparency of the films was enhanced under high temperature. It is also found that the saturation magnetization (M _s) of the films increases with the temperature. As the content of the Fe₂O₃ increases, when the content of the Fe₂O₃ is around 30wt%, the M _s of the films has a maximum value.