Modification of natural graphite using pitch through dynamical melt-carbonization

The graphite was modified using pitch through dynamical melt-carbonization, and the effects of modification temperature and the amount of pitch on the characteristics of graphite were investigated. The structure and characteristics of the graphite were determined by X-ray diffractometry(XRD), scanning electron microscopy(SEM), particle size analysis and electrochemical measurements. The results show that the modified graphite has a disordered carbon/graphite composite structure, larger average particle diameter, greater tap density, and better electrochemical characteristics than the untreated graphite. The sample coated with 10% pitch dynamical melt-carbonized at 400 ℃ for 3 h and heat-treated at 850 ℃ for 2 h has better electrochemical performances with a reversible capacity of 360.5 mA·h/g, a irreversible capacity of 41.0 mA·h/g, and an initial coulombic efficiency of 89.8% compared with natural graphite and disordered carbon. The cycling stability of the Li/C cell with modified graphite as anodes is improved, and its capacity retention ratio at the 30th cycle is up to 94.37%.     

Bi2S3-MoS2/石墨烯复合材料的合成及电化学储锂性能

为了研发高性能的锂离子电池负极材料,采用水热法合成了Bi₂S₃-MoS₂/石墨烯复合材料,利用X-射线衍射（XRD）、扫描电镜（SEM）、高分辨透射电镜（HRTEM）、热重分析（TGA）和X-射线光电子能谱（XPS）对复合材料进行表征,讨论复合材料的微观结构对电化学储锂性能的影响. 特别是,当Bi与Mo的物质的量之比为1∶4时,Bi₂S₃-MoS₂/石墨烯的电化学储锂可逆比容量可以达到1 140 mA·h/g,并具有稳定的循环性能. 当充放电电流密度为1 000 mA/g时,其高倍率特性为886 mA·h/g. Bi₂S₃-MoS₂/石墨烯复合材料优异的电化学储锂性能主要由于MoS₂具有更少的层数和较多的边缘以及Bi₂S₃纳米粒子具有更均匀的粒径,并能很好地分散在石墨烯表面,增强了复合材料容纳锂离子的能力,改善了储锂电极过程的动力学性能.     

Electrochemical performance of LiFePO4/（C＋Fe2P） composite cathode material synthesized by sol-gel method

A LiFePO4/(C+Fe2P) composite cathode material was prepared by a sol-gel method using Fe(NO3)3·9H2O,LiAc·H2O,NH4H2PO4 and citric acid as raw materials,and the physical properties and electrochemical performance of the composite cathode material were investigated by X-ray diffractometry(XRD),scanning electron microscopy(SEM),transmission electron microscopy(TEM) and electrochemical tests.The Fe2P content,morphology and electrochemical performance of LiFePO4/(C+Fe2P) composite depend on the calcination tempera...     

层状磷酸锆的制备及插层研究

具有层状结构的磷酸锆α-Zr（HPO4）2·H2O通过粉末X-射线衍射（XRD）,振动光谱（红外IR和拉曼光谱Raman）,热分析仪（TG）,透射电子显微镜（TEM）,扫描电子显微镜（SEM）和BET氮气吸附等手段进行了表征.所制备的α-Zr（HPO4）2·H2O的BET表面积为12.29 m^2/g.研究了α-Zr（HPO4）2·H2O的插入行为,与四甲基溴化铵和十六烷基三甲基溴化铵的插入反应表明插入是完全的,层间距分别增加了0.46 nm和1.68 nm,且插入化合物的荧光性质在室温被检测.     

Carbonized Zn-MOF/PANI的合成及其电容性能研究

通过简单的方法将煅烧过的金属有机框架(MOF)与聚苯胺(PANI)复合,形成了简单的MOF/PANI复合材料.通过X射线衍射(XRD)、扫描电子显微镜(SEM)、傅立叶转换红外线光谱(FTIR)对其进行了表征,并用循环伏安法(CV)对其电化学性能进行了测试.结果证明了MOF/PANI的比容量在电流密度为1 A/g下可高达477 F/g.     

Synthesis and characterization of triclinic structural LiVPO4F as possible 4.2 V cathode materials for lithium ion batteries

A potential 4.2 V cathode material LiVPO4F for lithium batteries was prepared by two-step reaction method based on a carbon-thermal reduction （CTR） process. Firstly, V2O5, NH4H2PO4 and acetylene black are reacted under an Ar atmosphere to yield VPO4. The transition-metal reduction is facilitated by the CTR based on C→CO transition. These CTR conditions favor stabilization of the vanadium as V^3＋ as well as leaving residual carbon, which is useful in the subsequent electrode processing. Secondly, VPO4 reacts with ElF to yield LiVPO4F product. The property of the LiVPO4F was investigated by X-ray diffractometry （XRD）, scanning electron microscopy （SEM） and electrochemical measurement. XRD studies show that LiVPO4F synthesized has triclinic structure（space group p I ）, isostructural with the naturally occurring mineral tavorite, EiFePO4-OH. SEM image exhibits that the particle size is about 2μm together with homogenous distribution. Electrochemical test shows that the initial discharge capacity of LiVPO4F powder is 119 mA·h/g at the rate of 0.2C with an average discharge voltage of 4.2V （vs Ei/Li^＋）, and the capacity retains 89 mA·h/g after 30 cycles.     

Hydrothermally Synthesizing Nanospheres of Pd Loaded TiO<Subscript>2</Subscript> for Photocatalytically Reducing CO<Subscript>2</Subscript> in Isopropanol to Isopropyl Formate

Photocatalytic reduction of CO₂ was carried out on villiform spherical catalysts of Pd-TiO₂ in isopropanol solution. The catalysts were synthesized by hydrothermal method, their structures, morphologies and optical absorption properties were characterized by X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM) and UV-vis absorption spectroscopy (UV-vis). The photocatalytic activities with different loading amounts and morphologies were evaluated for determining the dominant effect and optimizing the catalyst preparation. Based on a villiform spherical TiO₂ with the largest specific surface area in our experiments, we prepared a set of catalysts with various loading amounts of palladium and tested them by bubbling CO₂ through the slurry of catalyst and isopropanol. The highest formation rate of isopropyl formate was 276.6 μmol/g·cat/h. Eventually we proposed the reaction mechanism.     

钨酸铁的超声合成及表征

利用乙二醇为表面活性剂,通过超声合成方法成功制备了粒径均匀、分散性良好的微米级FeWO4。利用粉末XRD、SEM及FT-IR等手段对所制备的FeWO4进行了表征。制得的FeWO4被固定在玻碳电极表面制成FeWO4/CHIT/GCE复合电极,电化学测试发现该电极能够加速Fe(Ⅲ)和Fe(Ⅱ)氧化还原对间的电子转移。进一步在该电极表面固定牛血红蛋白(Hb)后,即得到一种新型的可用于测定溶液中H2O2浓度的传感器。该传感器线性范围为5.0至460μmol·L-1,检测限为1.0μmol·L-1(3σ)。     

碳化棉织物作为微生物燃料电池廉价阳极材料的研究

使用廉价的日常废棉纺织物作为原材料,通过碳化处理制备了一种新颖的、生物相容性的、多孔的、高导电性的、低成本的碳化棉织物（CCTs）电极,并且用于微生物燃料电池（MFCs）的阳极材料.采用场发射扫描电子显微镜（FESEM）,X射线衍射（XRD）,拉曼光谱（Raman）,傅里叶变换红外光谱（FTIR）,X射线光电子能谱（XPS）和Brunauer-Emmett-Teller （BET）等方法进行表征.表征结果显示,CCT-1000电极的表面比较粗糙,比表面积为209.64 m²·g^–1,大大增强了电极与细菌之间的相互作用,从而增加了细菌在电极上的负载量,促进了细菌胞外电子传递（EET）.使用CCT-1000阳极的MFC的输出功率为738±20 mW·m^–2,比使用商业碳毡阳极的MFC的输出功率提高了43%.另外充分利用廉价的废棉纺织物,可以大大降低MFCs的成本,同时减少环境污染问题.     

Influences of melt spinning on electrochemical hydrogen storage performance of nanocrystalline and amorphous Mg2Ni-type alloys

In order to improve the electrochemical hydrogen storage performance of the Mg₂Ni-type electrode alloys, Mg in the alloy was partially substituted by La, and the nanocrystalline and amorphous Mg₂Ni-type Mg_20−x La _x Ni₁₀ (x=0, 2) alloys were synthesized by melt-spinning technique. The microstructures of the as-spun alloys were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The electrochemical hydrogen storage properties of the experimental alloys were tested. The results show that no amorphous phase is detected in the as-spun Mg₂₀Ni₁₀ alloy, but the as-spun Mg₁₈La₂Ni₁₀ alloy holds a major amorphous phase. As La content increases from 0 to 2, the maximum discharge capacity of the as-spun (20 m/s) alloys rises from 96.5 to 387.1 mA·h/g, and the capacity retaining rate (S ₂₀) at the 20th cycle grows from 31.3% to 71.7%. Melt-spinning engenders an impactful effect on the electrochemical hydrogen storage performances of the alloys. With the increase in the spinning rate from 0 to 30 m/s, the maximum discharge capacity increases from 30.3 to 135.5 mA·h/g for the Mg₂₀Ni₁₀ alloy, and from 197.2 to 406.5 mA·h/g for the Mg₁₈La₂Ni₁₀ alloy. The capacity retaining rate (S ₂₀) of the Mg₂₀Ni₁₀ alloy at the 20th cycle slightly falls from 36.7% to 27.1%, but it markedly mounts up from 37.3% to 78.3% for the Mg₁₈La₂Ni₁₀ alloy.     

Synthesis and characterization of VO<Subscript>2</Subscript>/mesoporous carbon composites for hybrid capacitors

VO₂/ordered mesoporous carbon (CMK-3) composites were prepared by solid-state reaction process. The microstructures were characterized by X-ray diffraction (XRD), nitrogen adsorption and desorption, field-emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). The experimental results showed that the vanadium oxide in the composites was vanadium dioxide (VO₂) with monoclinic structure, which was artificially loaded on the outer surface of CMK-3. VO₂/ordered mesoporous carbon composites present a significantly improved capacitive performance (131 F/g) increased by 40.86% compared to that of CMK-3 carbon (93 F/g). Therefore, as-prepared VO₂/mesoporous carbon composites suggest promising applications in hybrid capacitors.     

Effect of Adding Microwave Absorber on Structures and Properties of Hypercoal-Based Activated Carbons

Using lignite-based hypercoal as raw material,KOH as activator and CuO as microwave absorber,we prepared hypercoal-based activated carbons by microwave-assisted activation.The pore structure and the electrochemical performance of the activated carbons were tested,and the effects of adding CuO in the activation reaction process were also investigated.The activated carbons prepared were characterized by nitrogen adsorption-desorption,X-ray diffraction (XRD) and scanning electron microscopy (SEM).The specific surface area and mesoporous ratio of the hypercoal-based activated carbon are 1 257 m~2/g and 55.4%,respectively.When the activated carbons are used as the electrode materials,the specific capacitance reaches 309 F/g in 3 M KOH electrolyte.In comparison with those prepared without CuO absorber,the specific capacitance increases by 11.6%.It was proved that the addition of microwave absorber in microwave-assisted activation was a low-cost method for rapidly preparing activated carbon,and it could effectively promote the development of the pore structure and improve its electrochemical performance.     

Synthesis and characterization of high-voltage cathode material LiNi0.5Mn1.5O4 by one-step solid-state reaction

LiNi_0.5Mn_1.5O₄ was prepared under various conditions by one-step solid-state reaction in air and its properties were investigated by X-ray diffractormetry (XRD), scanning electron microscopy (SEM) and electrochemical measurement. XRD patterns show that LiNi_0.5Mn_1.5O₄ synthesized under various conditions has cubic spinel structure. SEM images exhibit that the particle size increases with increasing calcination temperature and time. Electrochemical test shows that the LiNi_0.5Mn_1.5O₄ calcined at 700 °C for 24 h delivers up to 143 mA · h/g, and the capacity retains 132 mA · h/g after 30 cycles. Foundation item: Project (76600) supported by Postdoctoral Science Foundation of Central South University     

Microwave-assisted synthesis of 3D flowerlike a-Ni(OH)_2 nanostructures for supercapacitor application

Three-dimensional flowerlike ?-Ni(OH)2 nanostructures were successfully synthesized by the microwave-assisted reflux as short as 30 min. The crystalline structure and morphology of the products were characterized by X-ray diffraction, N2 adsorption-desorption isotherms, field emission scanning electron microscopy, and transmission electron microscopy. The ?-Ni(OH)2 nanostructure shows a large surface area of 173 m2 g?1 and narrow mesopore distribution. The electrochemical properties of the as-prepared ?-Ni(OH)2 as an electrode material for supercapacitor were investigated by cyclic voltammetry and galvanostatic charge-discharge measurements in 6 mol/L KOH electrolyte. The ?-Ni(OH)2 nanostructure shows a maximum specific capacitance of 2030 F g?1 at a current density of 1 A g?1 and exhibits excellent rate capability. These results suggest that it is a promising electrode material for supercapacitor application.     

Synthesis and electrochemical performance of TiO2-B as anode material

TiO₂-B was synthesized by solid-state reaction. The structures, surface morphologies and electrochemical performances of TiO₂-B were characterized by X-ray diffractometry (XRD), scanning electron microscopy (SEM) and electrochemical measurement, respectively. The effects of calcining temperature, molar ratio of K₂O to TiO₂ and calcining time on the characteristics of TiO₂-B were investigated. The results show that the calcining time exerts a significant influence on the electrochemical performances of TiO₂-B. The TiO₂-B is obtained with good crystal structure and suitable size by using K₂Ti₄O₉, which is prepared at 950°C for 24 h under the condition of x(K₂O)/x(TiO₂)=1:3.5. The TiO₂-B delivers all initial discharge capacity of 231.6 mA·h/g. And the rate capacity is 73.2 mA·h/g at 1 675 mA/g, which suggests that TiO₂-B is a promising anode material for the lithium ion batteries.     

二氧化锰改性多壁碳纳米管吸附水中Sb(Ⅲ)

采用液相氧化还原法制备二氧化锰/多壁碳纳米管（MnO2/MWNTs）复合材料,利用X射线衍射仪（XRD）、扫描电镜（SEM）、透射电镜（TEM）、激光粒度仪和N2吸附-脱附对改性前后MWNTs的物化性能进行表征.通过对水中Sb(Ⅲ)的静态吸附试验考察改性碳纳米管的吸附容量,同时还考察pH值、锑的初始浓度、吸附剂投加量、吸附时间和温度对吸附效果的影响.结果表明,在Sb(Ⅲ)初始浓度为1.5 mg/L、吸附剂投加量为0.5 g/L、温度为298 K、pH值为2.00的条件下,二氧化锰改性后的碳纳米管对锑的去除率可达到97.72%,比未改性碳纳米管的去除率提高51.29%,吸附容量也从原始CNT的3.01 mg/g增大到6.00 mg/g.最后发现该吸附过程较好地符合Freundlich吸附等温线,pH值对吸附效果的影响较大.     

锂离子电池负极材料SnO2-Gn-C三元复合物的制备及其电化学性能

通过两步水热法合成了可用作锂离子电池负极材料的二氧化锡-石墨烯-炭（SnO2-Gn-C）三元复合物.采用X射线粉末衍射（XRD）、透射电镜（TEM）和电化学测试研究了SnO2-Gn-C复合物的晶型结构、形貌和电化学性能,并考察了反应温度和Sn/Gn物质的量比对复合物电化学性能的影响.实验结果显示,SnO2-Gn-C复合物在200mA· g-1电流密度下初始放电比容量达到1 225mA·h·g-1,50次充放电循环后比容量仍有约229mA.h·g-1.SnO2-Gn-C良好的电化学性能主要归结于大比表面积的石墨烯对SnO2纳米粒子的良好分散作用、石墨烯和炭的高导电性以及炭包覆后的复合物充放电时体积效应的显著减小.     

载锆颗粒活性炭吸附去除水溶液中的硫酸根离子

制备负载氧化锆的颗粒活性炭(Zr-GAC),以吸附水溶液中的硫酸根离子.采用扫描电镜(SEM)、X射线衍射(XRD)、X射线光电子能谱(XPS)和比表面积测定等方法对Zr-GAC进行表征.结果表明,Zr-GAC具有多孔的表面积,其上具有许多由氧化锆组成的团聚体.XPS分析证实,吸附剂表面存在大量的锆和羟基,氧化锆改性后...     

水热法制备Sb_2Se_3纳米晶

以酒石酸锑钾(K(SbO)C4H4O6.1/2H2O)和硒粉作为锑源和硒源,自制的2-十一烷基-1-二硫脲乙基咪唑啉季铵盐(SUDEI)为表面活性剂,150℃水热反应24 h,得到不同形貌的Sb2Se3纳米晶。通过透射电镜(TEM)、X射线衍射(XRD)、X射线光电子能谱仪(XPS)对Sb2Se3纳米晶进行了表征。讨论了反应条件对Sb2Se3纳米晶形貌的影响。     

UiO-66/C复合材料的制备及其吸附性能研究

采用溶剂热合成方法,制备了金属有机骨架材料UiO-66及其UiO-66/C复合材料,对所得产物样品进行XRD和SEM以及红外光谱测试表征。结果表明,所制备样品为纯相UiO-66材料,添加碳球未改变UiO-66的晶相结构。以亚甲基蓝和甲基橙模拟染料废水,对所制备的UiO-66及其UiO-66/C复合材料的吸附性能进行了评价。实验结果表明,添加胶态碳球可显著提高UiO-66对亚甲基蓝的吸附性能,吸附容量由30 mg/g提高到67mg/g,UiO-66对甲基橙表现出优异的吸附能力,吸附容量高达226 mg/g;吸附的动力学过程符合准二级动力学方程。