球磨微波法制备Li3V2（PO4）3/C及其电化学性能表征

本文采用球磨微波法合成锂离子电池正极材料Li3V2(PO4)3/C,并研究了微波辐射时间对样品电化学性能的影响.结果表明,640 W微波辐射18 min合成的材料,结晶度高,粒径小而均匀.该电极5C倍率下首次放电比容量达101.3 mAh·g-1,300周期循环,其放电比容量仍保持100.8 mAh·g-1,展示出良好的应用前景.     

锂离子电池负极材料Li4Ti5O12的半固相法制备及碳包覆改性

由半固相法制得锂离子电池负极材料Li4Ti5O12,并研究了Li4Ti5O12的碳包覆改性.采用XRD、SEM、TEM以及HRTEM观察和分析产物的相结构与形貌.采用恒流充放电、循环伏安法和交流阻抗技术测试了材料的电化学性质.结果表明,Li4Ti5O12因颗粒团聚电化学性能严重下降,该电极在0.1C和0.5C首周期放电容量分别为121.7和87.6 mAh·g-1;碳包覆Li4Ti5O12/C材料呈球形分布,能抑制颗粒团聚,该电极倍率<0.5C时的放电比容量大于180 mAh·g-1,超过Li4Ti5O12的理论放电比容量(175 mAh·g-1);在1C、5C和10C倍率下,其容量仍保持在136、79.9和58.3 mAh·g-1,碳包覆改性材料具有优异的循环寿命和高倍率性能.     

一种新的流变相法制备锂离子电池纳米-LiVOPO_4正极材料(英文)

采用新型流变相法制备锂离子电池正极材料纳米-LiVOPO4.采用X射线衍射、扫描电子显微镜以及电化学测试等手段对LiVOPO4的微观结构、表面形貌和电化学性能进行了表征.结果表明,采用流变相法制备的LiVOPO4由粒径大约在10-60nm的小颗粒组成.首次放电容量,首次充电容量以及库仑效率分别为135.7mAh·g-1,145.8mAh·g-1和93.0%.0.1C(1C=160mA·g-1)放电时,60次循环后,放电容量保持在134.2mAh·g-1,为首次放电容量的98.9%,平均每次循环的容量损失仅为0.018%.而1.0C和2.0C放电时的放电容量达到0.1C放电容量的96.5%和91.6%.随着放电次数的增加,电荷转移阻抗增加,而锂离子在电极中的扩散系数达到10-11cm2·s-1数量级.实验结果显示采用流变相法制备的LiVOPO4是一种容量高、循环性能好、倍率性能好的锂离子电池正极材料.     

酚醛树脂包覆氧化天然石墨作为锂离子电池负极材料

天然石墨经过浓硫酸氧化处理,酚醛树脂包覆并高温碳化后形成具有核壳结构的碳包覆氧化天然石墨复合材料.采用扫描电子显微镜(SEM),透射电子显微镜(TEM),X射线衍射(XRD),激光显微拉曼光谱(Raman)等检测技术对氧化处理以及酚醛树脂热解碳包覆前后天然石墨材料的结构与形貌进行分析与表征.结果表明,氧化处理与适量的酚醛树脂热解碳包覆有效修复了天然石墨表面的一些缺陷结构,使其表面更为光滑.电化学测试结果显示,经过氧化处理与酚醛树脂热解碳包覆后天然石墨材料电化学性能得到明显提高.酚醛树脂包覆量为9%时,复合材料表现出最好的电化学性能,其首次放电比容量为434.0mAh·g-1,40次循环后,放电比容量保持在361.6mAh·g-1,而未经处理的天然石墨放电比容量仅为332.3mAh·g-1.该改性方法有效提高了天然石墨材料的比容量,对其进一步应用具有重要意义.     

多元醇还原法合成锂离子电池正极材料LiFePO_4

以三甘醇为还原剂,Li2CO3和三价铁源FePO4为原料,通过多元醇还原法在低于300℃下直接制备了结晶良好的纯相LiFePO4,无须后续热处理。0.1C首次放电比容量为140.5mAh·g-1。为了进一步改善纯相LiFePO4的电导率,以聚乙烯醇为碳源,在700℃下热处理进行了碳包覆改性,获得了LiFePO4/C复合正极材料。合成的LiFePO4/C在0.1C下放电容量为155mAh·g-1,5C倍率下放电比容量保持在125mAh·g-1,具有很好的倍率性能和循环稳定性。     

熔盐锌热法制备三维多孔碳用于高性能钾离子电池负极材料

采用熔盐锌热法,以蔗糖为前驱体成功制备了三维多孔碳材料,并将其用作钾离子电池负极材料。所制备的三维多孔碳具有大量相互贯通的孔道,有效地缓解了电极在充放电循环过程中的体积效应,提高了电解液对电极的浸润性,缩短了钾离子的扩散路径,从而展现出优异的循环稳定性和倍率性能。三维多孔碳电极在0.5 A·g-1的电流密度下,经过2500次循环后仍展现174.6 mAh·g-1的比容量,甚至在4.4 A·g-1的高倍率下容量仍保持在170 mAh·g-1。     

不同碳源对多孔球形LiFePO4/C复合材料的影响

采用喷雾干燥-碳热还原法(SDCTM),分别研究了无机和有机碳源对锂离子正极材料LiFePO4/C形貌、结构及其充放电性能的影响。结果表明:以无机碳源炭黑制备的LiFePO4/C呈不规则球形,一次颗粒粒径在800nm左右,比表面积为2m2·g-1,0.1C放电比容量为107.3mAh·g-1。而以有机碳源制备的LiFePO4/C,其形貌较为规则,呈多孔球形结构,具有较高的比表面积和放电比容量。其中,以柠檬酸为碳源制备的多孔球形LiFePO4/C复合材料,其孔径均在50nm左右,比表面积可达32m2·g-1;在室温下,0.1C和10C首次放电比容量分别为158.8和87.2mAh·g-1,具有优异的循环性能和高倍率充放电性能。     

粒径可控纳米LiFePO4/C的制备及其电化学性能研究

LiFePO4电极的倍率特性与材料的粒度和电子导电性有很大关系.采用共沉淀方法,调控预处理温度,将3种不同尺寸的FePO4前驱体通过表面修饰对-羟基苯甲酸的聚合物,可合成不同尺度的LiFePO4/C材料,分别为80 nm、200nm和1μm.纳米尺度LiFePO4-a/C电极,30C放电比容量达到了100 mAh·g-1,而微米级LiFePO4-c/C电极放电比容量仅为54mAh·g-1.均一碳包覆的LiFePO4/C电极表现出强抗氧化性,不仅提高其导电性,还可防止材料氧化.     

锂离子电池碳包覆锡负极性能研究

应用水热法分解葡萄糖制作锂离子电池碳包覆锡负极. 充放电测试表明,添加5%（by mass）乙炔黑导电剂的该电极初始放电比容量达967 mAh.g^-1,经50周循环其放电比容量仍保持362 mAh.g^-1,远高于锡电极的比容量（50周循环166 mAh.g^-1）. 碳包覆可防止锡粉团聚,降低锡的不可逆容量损失. 而添加乙炔黑可降低碳包覆电极与电解液间的交流阻抗,改善电极内部锂离子及电子的传导通道,从而也提高了该电极的初始放电比容量.     

水溶-蒸发法制备LiFePO4/C及其电化学性能研究

由LiH2PO4和FeC2O4.2H2O作原料、柠檬酸为碳源,用水溶-蒸发法制备了LiFePO4/C正极样品.采用X射线衍射(XRD)、扫描电镜(SEM)和透射电镜(TEM)分析、观察样品.用充放电曲线和电化学交流阻抗(EIS)谱图测试LiFePO4/C电极.结果表明,700℃焙烧的LiFePO4/C样品(碳量3.03%,by mass)结晶度高、无杂相、颗粒粒径100 nm,其表面包覆约5 nm碳层.该电极0.5C、2C、5C和10C(1C=170 mA.g-1)倍率放电,其比容量分别为148.2 mAh.g-1、142.4 mAh.g-1、127.4 mAh.g-1和108.5 mAh.g-1,循环寿命曲线稳定.     

利用手持技术改进测定乙醇分子结构实验

利用压强传感器代替排水集气法,改进测定乙醇分子结构实验的仪器装置,并探索最佳反应条件。另外,设计两个空白实验,结合压强变化曲线对实验误差进行相关讨论。     

Neutral diterpenoids of oleoresins of five species of conifers of Transcarpathia

The compositions of the neutral diterpenoids of the oleoresins of five species of conifers growing in the Transcarpathia have been studied. It has been found that the oleoresins ofAbies alba M.,Larix decidua M., andPicea excelsa L. contain more than 50% of neutral diterpenoids. The group and qualitative compositions of the oxygen-containing diterpenoids have been determined. In the oleoresins ofAbies alba,Picea excelsa, andPicea abies tertiary alcohols — cis-abienol and isocembrol — predominate, while inLarix decidua the main component is the hydroxy ester larixyl acetate. Primary alcohols related to the resin acids have been found in all the oleoresins investigated. Features of the distribution of diterpenoids according to the species of conifers have been revealed. The results obtained are necessary for the chemotaxonomy of conifers of the family Pinceae.Novosibirsk Institute of Organic Chemistry, Siberian Branch, Academy of Sciences of the USSR. Translated from Khimiya Prirodynkh Soedinenii, No. 6, pp. 812–816, November–December, 1988.     

物质分配系数的测定实验改进

实验教学目的是从解决实际问题出发,以实验技术训练和实验设计思想培养为目标。介绍了将单一的物质分配系数测定实验改进为综合实验,提高了实验效果及实验资源利用率。     

光谱仪测试范围的扩展

由于石化行业的生产需要，其材质的使用具有多样性和广泛性，经常会出现顾客委托的测试样品的一个或几个元素跨越光谱仪现有测试程序测量范围的情况。本法通过对光谱仪测试原理的认识，根据光谱仪的测试能力及标样的采集，实现了一个或几个元素测量范围的扩展，并对其测量的影响因素进行了研究。     

Dichroism of absorption and polarization of phosphorescence of molecules of the closed form of nitrobenzospirothiopyran

The spectral-polarization characteristics of absorption and phosphorescence of molecules of the initial form of nitro-substituted indolinospirobenzothiopyran were studied in oriented polyethylene films and in solutions with different polarity. An oscillator model of the electron transitions responsible for the formation of absorption and luminescence spectra was suggested. It was established that the principal differences in the spectral and photophysical properties of the compound studied and its oxygen-containing analog are associated with the fact that the electronegativity of the S atom is lower than that of the O atom. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 6, pp. 1143–1146, June, 1997.     

Influence of viscosity of medium on processes of oxygen quenching of excited states of mesoporphyrin

The oxygen quenching rate constants for singlet and triplet excited states of the dimethyl ester of mesoporphyrin IX increase with decreasing viscosity of the medium and reach a maximum at a viscosity of approximately 0.4 mPa·sec, after which the rate constants begin to decrease. The drop in rate constant with increasing fluidity of the medium may be related to a nonequilibrium character of the elementary act in the interaction of the reactants in the solvent cage. In viscous media such as isopropyl alcohol, isobutyl alcohol, and isoamyl alcohol, the reaction radius is greater than the sum of the radii of the reacting particles. The long-range character of these processes is due to the relatively weak dependence of the quenching probability on distance.Translated from Teoreticheskaya i Éksperimental'naya Khimiya, Vol. 25, No. 2, pp. 161–167, March–April, 1989.     

Effect of the Method of Modification of Zeolite X on Selectivity of Catalytic Methylation of Toluene

Theoretical and Experimental Chemistry - The effect of the method of modification of catalysts based on zeolite X by cesium and magnesium cations (ion exchange and impregnation) on the selectivity...