Preparation of layered oxide Li（Co1/aNi1/3Mn1/3）O2 via the sol-gel process

To obtain homogenous layered oxide Li(Co1/3Ni1/3Ni1/3Mn1/3)O2 as a lithium insertion positive electrode material,the sol-gel process using citric acid as a chelating agent was applied.The material Li(Co1/3,Ni1/3Mn1/3)O2 was synthesized at different calcination temperatures.XRD experiment indicated that the hyered Li(Co1/3Ni1/3Mn1/3)O2material could he synthesized at a lower temperature of 800℃,and the oxidation state of Co,Ni,and Mn in the cathode confirmed by XPS were 3, 2,and 4,respectively.SEM observations showed that the synthesized material could form homogenous particle morphology with the particle size of about 200nm In spite of different calcination temperatures,the charge-discharge curves of all the samples for the initial cycle were similar,and the cathode synthesized at 900℃ showed a small irreversible capacity loss of 11.24% and a high discharge capacity of 212.2 mAh.g-1 in the voltage range of 2.9-4.6 V.     

Effect of calcination temperature on characteristics of LiNi1/3Co1/3Mn1/3O2 cathode for lithium ion batteries

LiNi1/3Co1/3Mn1/3O2 was synthesized by sol-gel method and effect of calcination temperature on characteristics of LiNi1/3Co1/3Mn1/3O2 cathode was investigated. The structure and characteristics of LiNi1/3Co1/3Mn1/3O2 were determined by XRD, SEM and electrochemical measurements. The results show that the compound LiNi1/3Co1/3Mn1/3O2 has layered structure with hexagonal lattice. With the increase of calcination temperature, the basicity of the material decreases, and the size of primary particle rises. The LiNi1/3Co1/3Mn1/3O2 calcined at 900 ℃ for 12 h shows excellent electrochemical performances with large reversible specific capacity of 157.5 mA-h/g in the voltage range of 2.75-4.30 V and good capacity retention of 94.03% after 20 charge/discharge cycles. Capacity of LiNi1/3Co1/3Mn1/3O2 increases with enhancement of charge voltage limit, and specific discharge capacities of 179.4 mA.h/g, 203.1 mA.h/g are observed when the charge voltages limit are fixed at 4.50 V and 4.70 V, respectively.     

Sintering behavior of aluminum nitride powder prepared by self-propagating high-temperature synthesis method

Fully dense aluminum nitride(AIN) ceramics were synthesized by self-propagating high-temperature synthesis(SHS) method using AIN powder as raw material with Y_2 O_3 additive. The sintering behavior was studied at different sintering temperatures and additive contents. The change of phase compositions, secondary phase distributions and grain morphologies during sintering process were investigated. It is shown that fully dense ceramics using AIN powder prepared by SHS method can be obtained when the sintering temperature is above 1830 ℃. Both Y_2 O_3 content and sintering temperature have an important influence on the formation of Y-Al-O phase and grain shape. When Y_2 O_3 content is identified, the grain morphology converts from polyhedron into sphere-like shape with the rise of sintering temperature. At a certain sintering temperature,the grain size decreases with the increase in Y_2 O_3 content. The influencing mechanisms of different YAl-O secondary phases and sintering temperatures on the grain size and morphology were also discussed based on the experimental results.     

FePO_4-coated Li[Li_(0.2)Ni_(0.13)Co_(0.13)Mn_(0.54)]O_2 with improved cycling performance as cathode material for Li-ion batteries

Li[Li_(0.2)Ni_(0.13)Co_(0.13)Mn_(0.54)]O_2 cathode materials were synthesized by carbonate-based co-precipitation method, and then, its surface was coated by thin layers of FePO_4. The prepared samples were characterized by X-ray diffraction(XRD), field emission scanning electron microscope(FESEM), energy-dispersive spectroscopy(EDS), and transmission electron microscopy(TEM). The XRD and TEM results suggest that both the pristine and the coated materials have a hexagonal layered structure, and the FePO_4 coating layer does not make any major change in the crystal structure. The FePO_4-coated sample exhibits both improved initial discharge capacity and columbic efficiency compared to the pristine one. More significantly, the FePO_4 coating layer has a much positive influence on the cycling performance. The FePO_4 -coated sample exhibits capacity retention of 82 % after 100 cycles at 0.5 ℃ between 2.0 and 4.8 V, while only 28 % for the pristine one at the same charge-discharge condition. The electrochemical impedance spectroscopy(EIS) results indicate that this improved cycling performance could be ascribed to the presence of FePO_4 on the surface of Li[Li_(0.2)Ni_(0.13)Co_(0.13)Mn_(0.54)]O_2 particle, which helps to protect the cathode from chemical attacks by HF and thus suppresses the large increase in charge transfer resistance.     

Phase Structure and Electrochemical Properties of Melt-Spun La_4MgNi_(17.5)Mn_(1.5) Hydrogen Storage Alloys

The(La_4MgNi_(17.5)Mn_(1.5))alloys at different melt-spun speeds were prepared by using a vacuum melt-spun furnace,and the phase structure and electrochemical properties of alloys were studied.X-ray diffraction analysis results show that melt-spun La_4Mg Ni_(17.5)Mn_(1.5)alloys are composed of CeCu_5-type,Pr_5Co_(19)-type and Ce Ni_2-type phase.As the melt-spun speed increased,the phase abundance of CeCu_5-type increased,but that of Pr_5Co_(19)-type decreased.Scanning electron microscopy–energy-dispersive spectroscopy analysis results show that melt-spun treatment can refine grain and make the alloys homogenization.Electrochemical tests show that all alloys have good activation performance within four cycles.With the increase in melt-spun speed,the cycle stability(S)of the alloys was improved obviously.After 100 cycles,the retention rate(S_(100))of the alloy increased from 54.82%(as-cast)to 82.29%(25 m/s).Nevertheless,the maximum discharge capacity(C_(max))and high-rate dischargeability gradually decreased.     

Study on rare earth/alkaline earth oxide-doped CeO2 solid electrolyte

Five types of rare earth/alkaline earth oxide-doped CeO2 superfine-powders were synthesized by a low-temperature combustion technique. The relevant solid electrolyte materials were also sintered by pressureless sintering at different temperatures. The results of X-ray diffraction and transmission electron microscopy showed that the grain size of the powders was approximately 20-30 nm, and rare earth/alkaline earth oxides were completely dissolved into ceria-based solid solution with fluorite structure. The electrical conductivities of the SmzO3-CeO2 system were measured by the ac impedance technique in air at temperatures ranging from 513-900℃. The results indicated that the ionic conductivities of Srno.2oCe0.8Ol.875 solid electrolyte increase with increasing sintering temperature, and the relationship between the conductivities and measuring temperature obeys the An＇henius equation. Then the SmzO3-CeO2 material was further doped with other rare earth/alkaline earth oxide, and the conductivities improve with the effective index.     

Synthesis and properties of Na_(0.8)Ni_(0.4)Mn_(0.6)O_2 oxide used as cathode material for sodium ion batteries

A new P2-structured oxide Na_(0.8)Ni_(0.4)Mn_(0.6)O_2 was synthesized using a solid reaction method in which Na_2 CO_3, MnO_2 and NiO were used as starting materials.This oxide has a high amount of electrochemically active Ni and exhibits good electrochemical intercalation behavior of Na ions, including good rate capability and good cycle performance at both room temperature and elevated temperature. It displays two apparent voltage plateaus at about 3.6 and 3.3 V, and its discharge capacity reaches92 mAh·g~(-1) at 0.1 C in the voltage range of 2.0-4.0 V. At1.0 C, its discharge capacity reaches 85.3 mAh·g~(-1). After80 cycles at different current rates, the as-prepared sample exhibits good capacity retention. At elevated temperature of 55 ℃, the discharge capacity remains the same at low current rate of 0.1 C, but at high current rate of 1.0 C, the discharge capacity is a little lower than that at room temperature.     

Mechanical wet-milling and subsequent consolidation of ultra-fine Al2O3-（ZrO2＋3%Y2O3） bioceramics by using high-frequency induction heat sintering

Alumina/zirconia composites were synthesized by wet-milling technique and rapid consolidation with high frequency induction heat sintering(HFIHS). The starting materials were a mixture of alumina micro-powder (80%, volume fraction) and 3YSZ nano-powders (20%). The mixtures were optimized for good sintering behaviors and mechanical properties. Nano-crystalline grains are obtained after 24 h milling. The nano-structured powder compacts are then processed to full density at different temperatures by HFIHS. Effects of temperature on the mechanical and microstructure properties were studied. Al2O3-3YSZ composites with higher mechanical properties and small grain size are successfully developed at relatively low temperatures through this technique.     

Electrochemical characterization of AlPO_4 coated LiNi_(1/3)Co_(1/3)Mn_(1/3)O_2 cathode materials for high temperature lithium battery application

Aluminum phosphate(AlPO_4) was used to modify the surface of LiNi_(1/3)Co_(1/3)Mn_(1/3)O_2(NCM) cathode material.The surface structure and electrochemical properties of the coated materials were investigated by X-ray photoelectron spectroscopy(XPS) and electrochemical impedance spectroscopy(EIS).The results confirm the formation of aluminum-containing solid solution on the surface of NCM particles.An aluminum phosphate coating blocks the Li~+ insertion-extraction process in cells charged at high rates at room temperature,increasing surface film resistance and decreasing discharge capacity.However,an aluminum phosphate aids the formation of a stable solid electrolyte interface film on NCM surface and stabilizes the R_(ct) of cell as samples electrochemically cycled at 55℃.The electrochemical studies suggest that the initial columbic efficiency is significantly enhanced.An NCM sample coated with 1.0 wt% AlPO_4 delivers a higher discharge capacity and shows excellent capacity retention ability.     

Exchange bias on polycrystalline BiFeO_3/Co_2Fe(Al_(0.5)Si_(0.5)) heterostructures

Polycrystalline antiferromagnetic BiFeO_3(BFO)thin films were grown on Si/Si O_2/Ti/Pt(111) substrates by pulsed laser deposition and then ferromagnetic films Co_2Fe(Al_(0.5)Si_(0.5))(CFAS) by magnetron sputtering. After fabrication, the films were vacuum-annealed under a 0.1-T magnetic field at different temperatures from 150 to 500 °C.The exchange bias field can be tuned by the annealing temperature for the heterostructures, and the electric domain size can be controlled by the crystal grain size. A large exchange bias of about 5*10~(-3)T is observed in one of the samples. It can be speculated that the crystal grain sizes are the key element in determining the exchange bias and coercivity of the films annealed at the temperature of higher than Neel temperature(T N) of BFO. Furthermore, it is possible to extend spin theories from single-crystal BFO system to polycrystalline BFO system.     

Synthesis of LiNi1/3CO1/3Mn1/3O2 cathode material via oxalate precursor

Using oxalic acid and stoichiometrically mixed solution of NiCl2, CoCl2, and MnCl2 as starting materials, the triple oxalate precursor of nickel, cobalt, and manganese was synthesized by liquid-phase co-precipitation method. And then the LiNi1/3Co1/3Mn1/3O2 cathode materials for Li-ion battery were prepared from the precursor and LiOH-H2O by solid-state reaction. The precursor and LiNi1/3Co1/3Mn1/3O2 were characterized by chemical analysis, XRD, EDX, SEM and TG-DTA. The results show that the composition of precursor is Ni1/3Co1/3Mn1/3C2O4·2H2O. The product LiNi1/3Co1/3Mn1/3O2, in which nickel, cobalt and manganese are uniformly distributed, is well crystallized with a-NaFeO2 layered structure. Sintering temperature has a remarkable influence on the electrochemical performance of obtained samples. LiNi1/3Co1/3Mn1/3O2 synthesized at 900 ℃ has the best electrochemical properties. At 0.1C rate, its first specific discharge capacity is 159.7 mA·h/g in the voltage range of 2.75-4.30 V and 196.9 mA·h/g in the voltage range of 2.75-4.50 V; at 2C rate, its specific discharge capacity is 121.8 mA·h/g and still 119.7 mA·h/g after 40 cycles. The capacity retention ratio is 98.27%.     

Effects of precipitator on the morphological, structural and electrochemical characteristics of Li[Ni1/3Co1/3Mn1/3]O2 prepared via carbonate coprecipitation

Three precipitators, i.e. Na₂CO₃, (NH₄)₂CO₃ and NH₄HCO₃, are employed to prepare Li[Ni_1/3Co_1/3Mn_1/3]O₂ via the carbonate coprecipitation method. The effects of precipitator on the morphological, structural and electrochemical characteristics of the prepared samples are studied. The sample prepared by using Na₂CO₃ as precipitator has irregular particle shape and nonuniform particle size, while the sample prepared by using (NH₄)₂CO₃ as precipitator has spherical particle shape and uniform particle size. Among all the samples, the one prepared with (NH₄)₂CO₃ exhibits the best hexagonal layered structure, which results in its highest discharge capacity and best cycling performance. Therefore, precipitator plays an important role in the coprecipitation reaction and makes a great impact on the characteristics of Li[Ni_1/3Co_1/3Mn_1/3]O₂.     

Effects of synthesis conditions on the structural and electrochemical properties of layered LiNi1/3Co1/3Mn1/3O2 cathode material via oxalate co-precipitation method

The uniform layered LiNi_1/3Co_1/3Mn_1/3O₂ cathode material for lithium ion batteries was prepared by using (Ni_1/3Co_1/3Mn_1/3)C₂O₄ as precursor synthesized via oxalate co-precipitation method in air. The effects of calcination temperature and time on the structure and electrochemical properties of the LiNi_1/3Co_1/3Mn_1/3O₂ were systemically studied. XRD results revealed that the optimal calcination conditions to prepare the layered LiNi_1/3Co_1/3Mn_1/3O₂ were 950°C for 15 h. Electrochemical measurement showed that the sample prepared under the such conditions has the highest initial discharge capacity of 160.8 mAh/g and the smallest irreversible capacity loss of 13.5% as well as stable cycling performance at a constant current density of 30 mA/g between 2.5 and 4.3 V versus Li at room temperature.     

Surface modification of LiNi<Subscript>1/3</Subscript>Co<Subscript>1/3</Subscript>Mn<Subscript>1/3</Subscript>O<Subscript>2</Subscript> with Cr<Subscript>2</Subscript>O<Subscript>3</Subscript> for lithium ion batteries

Cr 2 O 3-coated LiNi 1/3 Co 1/3 Mn 1/3 O 2 cathode materials were synthesized by a novel method. The structure and electrochemical properties of prepared cathode materials were measured using X-ray diffraction (XRD), scanning electron microscopy (SEM), charge-discharge tests, cyclic voltammetry (CV), and electrochemical impedance spectroscopy (EIS). The measured results indicate that surface coating with 1.0 wt% Cr 2 O 3 does not affect the LiNi 1/3 Co 1/3 Mn 1/3 O 2 crystal structure (α-NaFeO 2 ) of the cathode material compared to the pristine material, the surfaces of LiNi 1/3 Co 1/3 Mn 1/3 O 2 samples are covered with Cr 2 O 3 well, and the LiNi 1/3 Co 1/3 Mn 1/3 O 2 material coated with Cr 2 O 3 has better electrochemical performance under a high cutoff voltage of 4.5 V. Moreover, at room temperature, the initial discharging capacity of LiNi 1/3 Co 1/3 Mn 1/3 O 2 material coated with 1.0 wt.% Cr 2 O 3 at 0.5C reaches 169 mAh·g 1 and the capacity retention is 83.1% after 30 cycles, while that of the bare LiNi 1/3 Co 1/3 Mn 1/3 O 2 is only 160.8 mAh·g 1 and 72.5%. Finally, the coated samples are found to display the improved electrochemical performance, which is mainly attributed to the suppression of the charge-transfer resistance at the interface between the cathode and the electrolyte.     

Synthesis and electrochemical properties of Li[NixCoyMn1-x-y]O2 （x, y= 2/8, 3/8） cathode materials for lithium ion batteries

The uniform layered Li(Ni_2/8Co_3/8Mn_3/8)O₂, Li(Ni_3/8Co_2/8Mn_3/8)O₂, and Li(Ni_3/8Co_3/8Mn_2/8)O₂ cathode materials for lithium ion batteries were prepared using the hydroxide co-precipitation method. The effects of calcination temperature and transition metal contents on the structure and electrochemical properties of the Li-Ni-Co-Mn-O were systemically studied. The results of XRD and electrochemical performance measurement show that the ideal preparation conditions were to prepare the Li(Ni_3/8Co_3/8Mn_2/8)O₂ cathode material calcined at 900°C for 10 h. The well-ordered Li(Ni_3/8Co_3/8Mn_2/8)O₂ synthesized under the optimal conditions has the I ₀₀₃/I ₁₀₄ ratio of 1.25 and the R value of 0.48 and delivers the initial discharge capacity of 172.9 mA·h·g⁻¹, the discharge capacity of 166.2 mA·h·g⁻¹ after 20 cycles at 0.2C rate, and the impedance of 558 Ω after the first cycle. The decrease of Ni content results in the decrease of discharge capacity and the bad cycling performance of the Li-Ni-Co-Mn-O cathode materials, but the decreases of Mn content and Co content to a certain extent can improve the electrochemical properties of the Li-Ni-Co-Mn-O cathode materials.     

丝网印刷氧化石墨烯对锂离子电池LiNi1/3Co1/3Mn1/3O2 三元正极的改性及性能影响

通过丝网印刷方法,在由LiNi_1/3Co_1/3Mn_1/3O₂、导电添加剂和聚偏氟乙烯制成的电极表面涂覆了一层薄薄的氧化石墨烯。在充电截止电压为4.3 V的条件下进行了循环性能和倍率性能测试。结果表明：未改性电极在恒电流充放电测试中容量下降且极化增加,而包覆改性后电极的容量衰减程度和极化增加速度降低。这是由于氧化石墨烯涂层抑制了LiNi_1/3Co_1/3Mn_1/3O₂电极和电解质之间的部分副反应,使得改性电极的循环稳定性和倍率性能显著提高,为提升LiNi_1/3Co_1/3Mn_1/3O₂电极性能提供了一种环境友好且非常有效的方法。     

Effect of a surface treatment for LiNi<Subscript>1/3</Subscript>Co<Subscript>1/3</Subscript>Mn<Subscript>1/3</Subscript>O<Subscript>2</Subscript> cathode material in lithium secondary batteries

LiNi_1/3Co_1/3Mn_1/3O₂ cathode material was surface-treated to improve its electrochemical performance. Al₂O₃ nanoparticles were coated onto the surface of LiNi_1/3Co_1/3Mn_1/3O₂ powder using a sol-gel method. The as-prepared Al₂O₃ nano-particle was identified as the cubic structure of Al₂O₃. XRD showed that the LiNi_1/3Co_1/3Mn_1/3O₂ structure was not affected by the Al₂O₃ coating. With a coating of 3 wt.% Al₂O₃ on LiNi_1/3Co_1/3Mn_1/3O₂, the cyclic-life performance and rate capability were improved. However, heavier coatings (5 wt.%) on LiNi_1/3Co_1/3Mn_1/3O₂ resulted in a considerable decrease of the discharge capacity and rate capability. The thermal stability of LiNi_1/3Co_1/3Mn_1/3O₂ materials was greatly improved by the 3 wt.% Al₂O₃ coating.     

Improved high-Q microwave dielectric resonator using ZnO-doped La(Co1/2Ti1/2)O3 ceramics

The microwave dielectric properties and the microstructures of ZnO-doped La(Co_1/2Ti_1/2)O₃ ceramics prepared by conventional solid-state route have been studied. Doped with ZnO (up to 0.75 wt%) can effectively promote the densification of La(Co_1/2Ti_1/2)O₃ ceramics with low sintering temperature. At 1320 °C, La(Co_1/2Ti_1/2)O₃ ceramics with 0.75 wt% ZnO addition possesses a dielectric constant (_r) of 30.2, a Q × f value of 73,000 GHz (at 8 GHz) and a temperature coefficient of resonant frequency (τ_f) of −35 ppm/°C.     

AlF3包覆锂离子电池正极材料Li1.2(Mn0.54Ni0.16Co0.08)O2的制备、表征及电化学性能（英文）

采用溶胶-凝胶法合成锂离子电池正极材料Li1.2(Mn0.54Ni0.16Co0.08)O2,并用Al F3对这种材料进行表面包覆改性。采用X射线衍射(XRD)、扫描电子显微镜(SEM)、高分辨率透射电子显微镜(HRTEM)等表征材料的结构和形貌。结果表明,合成的Li1.2(Mn0.54Ni0.16Co0.08)O2具有典型的层状α-Na Fe O2结构,AlF3均匀包覆在Li1.2(Mn0.54Ni0.16Co0.08)O2材料表面,包覆层厚度为5~7 nm。电化学测试表明,包覆Al F3后材料的电化学性能得到提高,在1C倍率下,包覆的AlF3材料的首次放电容量为208.2 m A·h/g,50次循环后容量保持率为72.4%,而未包覆AlF3的材料的首次放电容量和容量保持率分别为191.7 m A·h/g和51.6%。     

Effects of ZrO2 Coating on LiNi1/3Mn1/3Co1/3O2 Particle with Microwave Pyrolysis

In this paper, ZrO₂-coated LiNi_1/3Mn_1/3Co_1/3O₂ is successfully prepared by the microwave pyrolysis method. The structure and electrochemical properties of the ZrO₂-coated LiNi_1/3Co_1/3Mn_1/3O₂ are investigated using x-ray diffraction, AC impedance, and charge/discharge tests, indicating that the lattice structure of LiNi_1/3Co_1/3Mn_1/3O₂ is unchanged after the coating but the cycling stability is improved. As the coating amount is 2 wt.%, initial capacity of the coated LiNi_1/3Co_1/3Mn_1/3O₂ decreases slightly. However, the cycling stability increases remarkably over the cut-off voltages of 2.75~4.3 V and the capacity retention reaches 93.1% after 50 cycles. Electrochemical impedance spectra results show that the increase of charge transfer resistance during cycling is suppressed significantly by coating with ZrO₂.