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1.
纳米尖晶石LixMn2O4的制备与电化学性能表征   总被引:11,自引:0,他引:11  
Nano-spinel LixMn2O4(0.6 ≤x≤ 1.0) was synthesized by two steps of coprecipitation and calcination. The influences of calcination temperature, time and Li/Mn ratio on the crystal structure and the particle size of LixMn2O4 were investigated. It was shown that the higher the calcination temperature, the more complete the crystal structure, and the larger the particle size. Moreover, the influence of calcination time on the crystal structure was insignificant when it was more than 3h at 700℃. With the increase of x in LixMn2O4 in the range of 0.6~1.0, the d111 and lattice parameter a increased first and then decreased. The electrochemical properties of nano-spinel LiMn2O4 using as cathode material of lithium-ion battery were studied. The low discharge capacity might be due to the irreversible capacity loss brought by the large surface area and lattice vacancies of the nano-spinel.  相似文献   

2.
SrTiO3 nanorods were synthesized in cetanyl trimethyl ammonium bromide (CTAB) reverse microemulsion containing CTAB, n-hexanol, n-octane and water with Ba(OH)2 as reactants. The effects of different conditions such as ω00=nH2O/ nCTAB], aging time and the concentration of reactants on the formation of the nanorods were studied. Transmission electron microscope (TEM), electron diffraction (ED) and X-ray diffraction(XRD)were used to characterize the morphology and the structure of the synthesized nanorods. The results show that SrTiO3 nanorods with a length of 260~2 000 nm and a diameter of 50~100 nm belonging to single crystal are single cubic system. The molar ratio of Sr to Ti of products is 1.0 as determinded by ICP.  相似文献   

3.
郝仕油 《无机化学学报》2007,23(8):1477-1480
Nanometer Ce1-xLaxO2-δ solid solutions were synthesized by microwave-induced combustion process us-ing cerium nitrate hexahydrate, lanthanum nitrate hexahydrate and urea as raw materials. The process took only six minutes to obtain La2O3-doped CeO2 nanopowders. The nanopowders were characterized by XRD, Laser Raman spectrum , UV-Vis spectroscopy,field-emission scanning electron micrograph(FE-SEM)and TEM. The results revealed that the grain size of Ce1-xLaxO2-δ varied from 20 to 40 nm calculated by Scherer formula through the plane of (111), that oxygen vacancy was produced in the crystal lattices and the concentration of oxygen vacancy was increased with La doping, therefore the covalence of Ce-O bond was strenthened, which results in more intensive UV-C(200~280 nm)absorption. It can be seen from SEM that the porous appearance was obtained. Grain size is no more than 40nm observed from TEM.  相似文献   

4.
锂离子电池正极材料LiMn2O4的合成与晶体结构(英)   总被引:2,自引:0,他引:2  
Spinel LiMn2O4 powders were prepared using two-step synthesis method consisting of solid-state reaction method and citrate modified sol-gel method. The effects of the calcination temperature and the Li/Mn ratio of raw materials were studied on the physicochemical and electrochemical properties of the spinel LiMn2O4 powders, such as crystallinity, lattice constant and density. The title compound was characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Polycrystalline LiMn2O4 powers calcined at 750 ℃ were found to be composed of very uniformly-sized microcrystal with an average particle size of 300 nm. The improvement in electrochemical properties was mainly attributed to the process of re-grinding by absolute alcohol.  相似文献   

5.
纳米二氧化钛粉末的溶胶-凝胶法合成及晶相转化   总被引:25,自引:0,他引:25  
Nanosized TiO2 powder with anatase and rutile structures was synthesized by a sol-gel method using TiCl4 ethanol solution as a precursor.The grain size of TiO2 powder was about 63nm after the precursor was calcined at 600℃ for 2 hours .The experimental techniques of XRD,TEM and Particle Distribution were used to characterize the synthesized specimens. Various special effects were investigated for their contribution to crystal structure and the size of TiO2 powder .The formation of anatase as well as the rutile phase of TiO2 was indicted from the XRD when the reaction temperature was above 30℃ and when the sol was irradiated by infrared rays .However, an anatase TiO2 powder formed after the heat treatment of the dried gel in a temperature range from 300℃ to 500℃.Under the vacuum drying and with the calcined time below 3hours ,the anatase phase was gained .As well as with the increase of gelatinizing time, the anatase TiO2 powder was obtained.  相似文献   

6.
纳米Mn-Zn铁氧体的制备和研究   总被引:10,自引:0,他引:10  
Nanosize manganese zinc ferrites were fabricated by hydrothermal precipitation route using Fe2(SO4)3, ZnSO4·7H2O, MnSO4·H2O as material, then some calcinated at 500 ℃ and studied by XRD, TEM, IR and VSM. The results showed that the products were spinel crystal structure and uniformly sized nanoparticles (15~25 nm) with little aggregation. The analysis of IR showed that the superficial water can be eliminated, but that was embedded in crystal lattice can not be removed by calcinating. The effect Zn content x on the lattice (a) of nanosize Mn1-xZnxFe2O4 was also discussed. The lattice of nanosize Mn1-xZnxFe2O4 decreases with x increasing; and its value deviated the standard lattice (a0) of normal size manganese zinc ferrites. A lot of water was absorbed during the hydrothermal process owing to the large surface of nanosize particles. The change of magnetic properties of MnxZn1-xFe2O4 with x increasing was studied: nanosize MnxZn1-xFe2O4 particles synthesized by us exhibited peculiar magnetic properties curve with Zn content (x) increasing, Superparamagnetic behaviors of the synthesized ZnFe2O4 samples were confirmed by magnetic characterization, which can be explained by the difference between the distribution of the metal ions (Mn2+, Zn2+ and Fe3+) among the tetrahedral (A) and the octahedral (B) sites of nanosize ferrite and that of bulk ferrite.  相似文献   

7.
混合溶剂前体法制备纳米CuO粉体及其性能表征   总被引:10,自引:0,他引:10  
Nano-CuO was prepared by heating nano-Cu2(OH)2CO3 precursors in different calcination temperatures. The precursor was synthesized from water-alcohol mixed solution of Cu(Ac)2 using mixed solution of NaOH and Na2CO3as precipitants. XRD, FT-IR, TEM, TG-DTA and surface area measurement techniques were used to investigate the properties of the CuO powder. The results show that the spherical, well dispersed nano-CuO powder with the average size of 15 nm and higher catalytic activity for H2O2 decomposition was obtained at 300 ℃. With the increasing of calcination temperature, crystal of CuO grows up, agglomeration of the powder becomes heavier and catalytic activity decreases. FT-IR patterns revealed that the vibration fine structure of Cu-O bond in nano-CuO powder disappears and main absorption is red-shifted with the average size of nano-CuO reducing.  相似文献   

8.
吴燕  赵新华  马辉 《无机化学学报》2002,18(12):1245-1249
Zirconium tungsten oxyfluoride, ZrWO4F2, was firstly synthesized with the precursor route. The composition of the compound was determined by combining the results of ICP and XPS. The indexed powder X-ray diffraction pattern of this compound indicates that it is a pure phase, orthorhombic crystal system, space group D22=P2122 and a=15.32(2)?,b=13.877(7)?,c=8.42(2)?.Combining the results of the DTA-TGA curves from room temperature to 700℃ and XRD patterns in different temperatures the mechanism was revealed during the solid precursor (1) been heated to 700℃. The zirconium tungsten oxyfluoride was considered to be a metastable com-pound. The ascertaining of annealing time and temperature is the key of handling.  相似文献   

9.
Na掺杂对锆酸锂吸收CO2性能的影响   总被引:1,自引:0,他引:1       下载免费PDF全文
By using Li2CO3, ZrO2, and Na2CO3 as starting materials, sodium-doped Li2(1-x)Na2xZrO3 absorbents were prepared by high-temperature solid-state reaction. The crystal structure of the lithium zirconate material was analyzed using a X-ray powder diffractometer (XRD), the microstructure of all the samples was observed using the method of scanning electron microscopy (SEM) and the CO2-absorption ability of the lithium zirconate material was studied using a thermogravimetric analyzer (TG). It was found that Li2(1-x)Na2xZrO3 absorbent with x=0.02 possesses the best performance. As much as (25 ± 0.4)% (wt) of CO2 was absorbed by such an absorbent in an atmosphere consisting of 20% (wt) CO2 and 80% (wt) air at 500 ℃ within 3 h. After 10 cycles of absorption-desorption this absorbent lost only 0.9% of its CO2-absorption capacity. No remarkable change in particle size and pH was observed.  相似文献   

10.
化学浴沉积法制备高取向钒酸铋薄膜   总被引:1,自引:0,他引:1  
Highly oriented BiVO4 films were synthesized on glass substrates by modified chemical bath deposition (CBD). The influence of the deposition parameters as temperature and time of deposition on the rate of process and the quality of BiVO4 films was studied by XRD, Raman Spectroscopy and SEM. The film deposited at 90 ℃ for 12 h was dense and uniform. The BiVO4 thin film under this optimal depositing conditions was consisted of octagonal crystalline grains in a narrow size distribution with an average size of about 7 μm, showing a (004) preferential orientation.  相似文献   

11.
负载Ni催化剂上1,4-丁炔二醇加氢反应的载体效应研究   总被引:2,自引:2,他引:0  
制备了Ni负载量为15%的3种催化剂Ni/Al_2O_3、Ni/SiO_2、Ni/ZrO_2,考察了其在1,4-丁炔二醇加氢反应中的催化性能,结合XRD、H_2-TPR、H_2-TPD、N_2物理吸附等表征,研究了载体性质对催化剂1,4-丁炔二醇加氢性能的影响.结果表明,Ni/SiO_2催化剂上,由于Ni与SiO_2间弱的相互作用,Ni物种主要以大晶粒形式存在,产生大量弱吸附H_2物种,有利于低温下1,4-丁炔二醇加氢,在温度50℃,氢气压力1 MPa时,反应2 h可实现1,4-丁炔二醇的完全转化,1,4-丁烯二醇和1,4-丁二醇选择性分别达到68.1%与18.2%.Ni/Al_2O_3中Ni与载体间具有强相互作用,主要存在Ni-Al_2O_3界面或溢流到Al_2O_3载体表面的强吸附H_2物种,而Ni表面的弱吸附H_2物种较少,催化加氢活性明显降低.Ni/ZrO_2中由于还原过程中ZrO_2的迁移包裹作用,Ni表面低温吸附H_2物种最少,活性最低,1,4-丁炔二醇转化率仅为8.1%,主产物为1,4-丁烯二醇.  相似文献   

12.
采用氨蒸发诱导法成功制备出纳米结构LiNi1/3Co1/3Mn1/3O2正极材料,借助X射线衍射(XRD)分析、扫描电镜(SEM)、透射电镜(TEM)、高分辨率透射电镜(HRTEM)、能量分散谱(EDS)和比表面测试等表征手段及恒电流充放电测试研究了其晶体结构、微观形貌和电化学性能. 研究表明该方法制备出的材料具有良好的α-NaFeO2层状结构,阳离子混排程度低. 纳米片交错堆积而成核桃仁状形貌,片与片之间形成许多纳米孔,而且纳米片的侧面属于{010}活性面,能够提供较多的锂离子的脱嵌通道. 在室温下及3.0-4.6 V充放电范围内,该材料在电流密度为0.5C、1C、3C、5C和10C时放电比容量分别为172.90、153.95、147.09、142.16 和131.23mAh·g-1. 说明其具有优异的电化学性能,非常有潜力用于动力汽车等高功率密度锂离子电池中.  相似文献   

13.
A variety of indolyl-2/3-methylsulfides tethered with sensitive functionalities were oxidized to the corresponding sulfoxides using a hitherto unexplored HF/H2O2 system.  相似文献   

14.
电解Co-Ni-Mn合金制备LiCo1/3Ni1/3Mn1/3正极材料   总被引:1,自引:0,他引:1  
叶茂  周震  卞锡奎  阎杰 《无机化学学报》2006,22(11):2005-2010
由Co-Ni-Mn合金出发,采用电解方法合成了含3种过渡金属元素的前驱物,再利用该前驱物制备了锂离子二次电池正极材料LiCo1/3Ni1/3Mn1/3。XRD测试结果表明通过该方法制备的正极材料具有较好的层状结构,SEM测试则显示材料由规则形状的1 μm左右颗粒组成。通过XPS实验证明Co、Ni、Mn 3种过渡金属元素在该材料中的价态分别为+3,+2,+4。采用循环伏安法对材料的电化学行为进行了研究,表明该材料具有较好的充放电可逆性。该材料在150 mA·g-1电流下经过50周的恒电流充放循环后容量仍能保持在160 mAh·g-1。  相似文献   

15.
16.
Mn / Ce / La / Al2O3催化剂中锰物种的精细结构研究   总被引:3,自引:0,他引:3  
采用浸渍法制备了La、Ce助剂改性的γ-Al2O3负载锰氧化物催化剂,运用XANES、EXAFS、XRD、XPS和H2-TPR等方法对催化剂的结构进行了表征,探讨了助剂对于催化剂中高分散Mn物种的精细结构、分散状态和存在形式的影响,并与样品的CO氧化活性相关联。XANES和EXAFS结果表明,500 ℃焙烧的样品中Mn物种主要以超细Mn2O3微晶形式存在,该物种由于高度分散使其配位对称性显著降低,无长程有序结构。TPR结果表明,样品中存在3种不同分散状态的表面Mn物种,即较难还原的Mn3+-O-Al3+相互作用物种,尺寸相对较大的三维分散的Mn2O3微晶,以及二维高度分散的Mn物种,后者是CO氧化反应的主要活性相。虽然Ce的加入使Mn物种的分散度有所降低,但Ce与Mn物种间的相互作用弱化了Mn-O键,加速了反应过程中活性氧物种的传递,提高了氧化还原循环的效率。同时,La的加入进一步促进了Ce物种在载体表面的分散,加强了Ce物种与Mn物种间的相互作用及催化协同性。  相似文献   

17.
层状LiCo1/3Ni1/3Mn1/3O2正极材料的合成及电化学性能研究   总被引:13,自引:0,他引:13  
采用液相法在800 ℃空气中烧结20 h合成出层状LiCo1/3Ni1/3Mn1/3O2正极材料。通过XRD、IR、SEM、XPS和电化学性能测试考察了产物的组成、结构、形貌及电化学性能。结果表明,所合成的LiCo1/3Ni1/3Mn1/3O2为六方单相,层状结构发育完善;产物呈球形且粒度小,分布窄,平均粒径为0.3 μm。以1 mA·cm-2的电流密度,在2.7~4.3 V区间进行充放电测试,前4周的充放电比容量分别为168/160 mAh·g-1、169/162 mAh·g-1、165/160 mAh·g-1、163/158 mAh·g-1,循环性能优良。循环伏安实验表明,该材料在3.9 V附近出现了一对对称性好的氧化还原峰。  相似文献   

18.
利用二次干燥法和共沉淀法分别制备出了非球形的Ni1/3Co1/3Mn1/3OOH前驱体和球形Ni1/3Co1/3Mn1/3(OH)2前驱体, 并分别和LiNO3混合烧结合成高密度非球形和球形的锂离子正极材料Li(Ni1/3Co1/3Mn1/3)O2. XPS分析表明, 二次干燥法制备的非球形Ni1/3Co1/3Mn1/3OOH前驱体其过渡金属Ni, Co和Mn的价态分别是+2, +3和+4, 而共沉淀法制备的球形Ni1/3Co1/3Mn1/3(OH)2前驱体其各金属价态为+2; X射线衍射分析表明, 非球形的Ni1/3Co1/3Mn1/3OOH前驱体比球形的前驱体具有较高的活性, 能够在低温下合成出Li(Ni1/3Co1/3Mn1/3)O2, 而且制备的产物结晶度高, 具有规整的层状α-NaFeO2结构, 扫描电镜显示制备的非球形产物颗粒均匀, 颗粒间隙小, 振实密度高达2.95 g•cm-3, 远高于球形的振实密度2.35 g•cm-3; 充放电实验表明, 由非球形前驱体制备的Li(Ni1/3Co1/3Mn1/3)O2其充放电性能和循环性能以及体积比容量均高于球形正极材料.  相似文献   

19.
采用高温固相法合成出层状锂离子电池正极材料LiNi1/3Mn1/3Co1/3O2。通过XRD、ICP、SEM和电化学测试手段对产物的结构、组成、形貌及电化学性能进行了研究。XRD结果表明此方法合成的LiNi1/3Mn1/3Co1/3O2具有标准的α-NaFeO2型层状结构,SEM照片显示颗粒粒径大约在500 nm左右,粒径分布较窄。以20 mA·g-1电流密度放电,充放电电压在2.8~4.4 V之间,其首次放电比容量为170 mAh·g-1,40次循环容量保持率为85.3%。进一步加入石墨导电剂后,同样条件下首次放电比容量变为179 mAh·g-1,50次循环容量保持率为89.6%。容量衰减主要发生在前10次循环。XRD和SEM测试表明循环初期容量衰减的原因是由材料本体结构变化和界面反应共同作用的结果。  相似文献   

20.
邓辉  蒋新 《无机化学学报》2011,27(1):119-124
利用吸附法原位制备CuO/SiO2、CuO-Ag/SiO2纳米复合物,研究了不同吸附质体系中预负载的纳米Ag粒子对CuO的影响。结果表明:Ag粒子对CuO的影响因吸附质的不同而不同。以Cu(Ac)2为吸附质,纳米Ag几乎没有影响;以NaOH为吸附质,纳米Ag使得CuO的晶粒粒径增大。这一结果与铜物种对Ag晶粒粒径的影响规律完全不同。通过比较不同吸附质的吸附行为,Cu(OH)2与硅胶表面的相互作用被认为是导致这一现象的原因。  相似文献   

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