多孔Co3O4纳米片的制备及其电化学性能研究

采用溶剂热法制备片状Co(CO3)0.5(OH).0.11H2O前驱物,经400℃煅烧2 h即可得到多孔Co3O4纳米片.通过场发射扫描电镜(FESEM)和透射电镜(HRTEM)观测了纳米片的形貌,利用X射线衍射(XRD)分析了纳米片的结构,通过循环伏安、恒流充放电和交流阻抗测试了材料的电化学电容性能.结果表明:多孔Co3O4纳米片厚度约为50 nm,孔径主要分布在10 nm左右;0.5 A/g恒流充放电情况下,比容量高达707 F/g,当电流密度高达8 A/g时比容量依然高达547 F/g;同时,该材料循环1 000次后,容量保持率为97.4%.     

Sol-gel derived bioactive hydroxyapatite/titania composite films on Ti6Al4V

The composite films consisting of the titania gel impregnated with hydroxyapatite （HAP） submicron particles were prepared on commercial Ti6A14V plates processed by a sol-gel route. HAP powders were synthesized based on wet chemical precipitation method with Ca（NO3）2.4H2O and （NH4）2HPO4 as starting reagents. After being calcined at 900℃, HAP powders were ultrasonically scattered in ethanol to produce HAP sol. The titania sol was prepared using titanium （IV） isopropoxide {Ti[OCH（CH3）2]4} as precursor. Both the titania sol and the HAP/titania mixture were sequentially spin-coated on the substrates and calcined at various temperatures. The characteristics and mechanical adhesion of the composite films were investigated. The results show that the as-prepared films are dense, homogeneous, well-crystallized, and there is a good interfacial adhesion between the film and the substrate. The in vitro bioactivities of these films were discussed based on the analysis of the variations of Ca and P concentrations in the simulated body fluid and their surface morphologies against immersion time.     

硫化铋纳米晶的水热合成及表征

在低温水热条件下,以BiCl3、Na2S2O3（或Na2S、硫脲）为反应物,制备了硫化铋（Bi2S3）纳米晶.用X射线粉末衍射（XRD）、扫描电镜（SEM）及纳米粒度测定仪对样品的结构及形貌进行了表征分析.结果表明,所得样品为正交晶系的Bi2S3纳米晶,形貌主要为纳米棒;同时硫源、反应温度及反应时间会影响样品的粒径.     

Electronic Structure and Thermoelectric Properties of Na and Ni-doped Ca3Co2O6

The electronic structures of Ca3Co2O6, Na and Ni doped models were studied by the quantum chemical software of Cambride Serial Total Energy Package （CASTEP） that is based on deusity function theory （DFT） and psendo-potential. The electronic conductivity, seebeck coefficient, thermal conduetivity and figure of merit （Z） were computed. The energy band structure reveals the form of the impurity levels due to the substitutional imapurity in semiconductors. Na-doped model stunts the character of p-type semiconductor, but Xi-doped model is n-type semiconductor. The calculation results show that the electric conduetirity of the doped model is higher than that of the non-doped model, while the Seebeck coefficient and thermal conductivity of the doped model are lower than those of the non-doped one. Because of the great increase of the electric conductivity, Z of Na- doped model is enhanced and thermoelectric properties are improved. On the other hand, as the large decline of Seebeck coefficient, Z of Ni-doped model is less than that of the non-doped model.     

铬酸镁纳米晶的微波制备与表征

以聚乙烯醇、镁盐和铬盐为原料,采用微波法制备了严格计量比的铬酸镁纳米晶.原料中金属离子与聚乙烯醇单体的摩尔比为1:3,在2.45GHz及不同微波功率作用下,首先制得铬酸镁前驱体.在500℃以上煅烧前驱体一定时间后得到铬酸镁纳米晶.铬酸镁纳米晶的X射线衍射和透射电镜表征表明:微波法能够得到具有良好尖晶石结构的铬酸镁纳米晶,是一种极有前景的合成纳米复合氧化物的新方法.     

以硫酸锰为原料制备四氧化三锰的理论分析

对用硫酸锰为原料制备Ｍｎ３Ｏ４进行了热力学分析,确定了制备Ｍｎ３Ｏ４的主要工艺条件,并在确定的条件下制出了Ｍｎ３Ｏ４,该研究对Ｍｎ３Ｏ４的制备有一定的应用价值。     

钛酸铅（PT）粉体的快速合成与表征

选用甘油为溶剂,以醋酸铅、钛酸四丁酯为基体原料,采用金属有机物热分解(MOD)法,合成了铁电钛酸铅(PT)粉体,并通过XRD、TG/DTA、IR、SEM等手段表征了合成粉体的组成以及形貌.结果表明,合成的PT粉体纯度高,颗粒细小均匀.     

溶胶-凝胶法制备Tb_3Sc_2Al_3O_(12)纳米粉体的研究

以柠檬酸为螯合剂,采用溶胶-凝胶法制备TSAG纳米粉体。通过XRD、FTIR和SEM测试手段对不同pH值和不同煅烧温度下合成的粉体进行了表征。结果表明:当温度为1000℃、pH值为3.3~3.6时,可以合成纯度较高的TSAG相,分布均匀,平均粒子尺寸为23.25nm;且随着烧结温度的升高,其粒径不断增大。     

改进Sol-gel法合成LiFePO4正极材料及其电化学性能

为了获得颗粒均匀、细小和电化学性能优异的LiFePO4, 采用sol-gel方法并添加表面活性剂聚乙二醇(PEG)制备LiFePO4/C。制备样品分别用XRD和SEM进行表征,通过充放电和循环伏安测试电化学性能。结果表明,nPEG/nLFP=1∶1、600 ℃制得样品颗粒均匀,平均粒径约为100 nm,在2.0～4.0 V(vs. Li)范围内,15 mA/g电流密度下放电,首次放电比容量为158 mAh/g,是理论容量的92.9％。制备样品展现良好的倍率性能和循环性能。     

Preparation and characterization of copper-nickel bulk nanocrystals

Copper-nickel nanoparticle was directly prepared by flow-levitation method(FL) and sintered by vacuum sintering of powder(VSP) method. Several characterizations, such as transmission electron microscopy(TEM), scanning electron microscopy(SEM), X-ray diffraction(XRD), differential thermal analysis(DTA), and energy-dispersive X-ray spectroscopy(EDX) were used to investigate the prepared nanostructures. The results of the study show that FL method could prepare high purity Cu-Ni nanocrystals of uniform spheres with size distribution between 20 and 90 nm. After sintering the bulk nanocrystalline copper-nickel has obvious thermal stability and the surface Webster hardness increases with the rising sintering temperature. At the temperature of 900 ℃, the specimen shows higher surface Webster hardness, which is about two times of traditional materials. When the sintering temperature arrives at 1 000 ℃ the relative density of bulk nanocrystals can reach 97.86 percent. In this paper, the variation tendency of porosity, phase and particles size of bulk along with the changing of sintering temperature have been studied.     

溶胶-凝胶法制备纳米钛酸钡

以溶胶－凝胶法制备纳米钛酸钡粉体,利用价廉的重晶石为主要原料制备钡源,有效地克服了传统方法因采用有机钡盐或有机钛而导致的生产成本过高的缺点：研究结果表明,该方法可制备出高纯钛酸钡粉体,制备过程中三废排放物中基本不含有害物质,并可从母液中回收质量较高的副产品硝酸铵,具有产品质量高,原料来源广泛、价格低廉、工艺环保、节能等特点．     

溶胶-凝胶法合成Gd2O3:Eu纳米晶及荧光性质的研究

采用溶胶-凝胶法合成了Gd2O3:Eu纳米晶.利用X射线衍射,热重及差热分析和荧光光谱等测试手段对Gd2O3:Eu的结晶过程、发光性质进行了研究.XRD结果表明,合成的样品在550℃开始结晶,晶粒随着温度的升高而长大,发光光谱测试表明,宽的主激发峰是由Eu3 电荷迁移态吸收与Gd3 离子的的激发峰重叠而成,主发射峰为610nm,它们的强度随烧结温度的提高而增强.     

柠檬酸盐溶胶凝胶法合成Ca3Co2O6陶瓷粉末

Ca3Co2O6是一种很有潜力的氧化物热电材料。研究了柠檬酸盐溶胶凝胶法制备Ca3Co2O6氧化物粉末，并应用TG／DSC、XRD和sEM等方法进行了测试研究。干凝胶在700℃煅烧就可以生成片状的Ca3Co2O9晶体，随着煅烧温度的升高，在850℃保温2h的条件下，Ca3Co4O9可以全部转化为条状的Ca3Co2O6晶体。pH值、乙二醇的加入与煅烧温度是影响制备过程的主要因素。乙二醇的使用可以减轻团聚现象，有利于预烧阶段的自燃烧，对晶相的生成没有多大影响。     

Preparation and electrochemical properties of Co3O4/graphite composites as anodes of lithium ion batteries

Co3O4/graphite composites were synthesized by precipitation of cobalt oxalate on the surface of graphite and pyrolysis of the precipitate, and the effects of graphite content and calcination temperature on the electrochemical properties of the composites were investigated. The samples were characterized by thermogravimetry and differential thermal analysis (TG/DTA), X-ray diffractometry (XRD), scanning electron microscopy (SEM), cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS) and charge/discharge measurements. With increasing the graphite content, the reversible capacity of the Co3O4/graphite composites decreases, while cycling stability improves dramatically, and the addition of graphite obviously decreases the average potential of lithium intercalation/deintercalation. The reversible capacity of the composites with 50% graphite rises from 583 to 725 mAh/g as the calcination temperature increases from 300 to 500 ℃, and the Co3O4/graphite composites synthesized at 400 ℃ show the best cycling stability without capacity loss in the initial 20 cycles. The CV profile of the composite presents two couples of redox peaks, corresponding to the lithium intercalaction/deintercalation for graphite and Co3O4, respectively. EIS studies indicate that the electrochemical impedance decreases with increasing the graphite content.     

Sol—Gel Synthesis of Normal Spinel LiMn2O4 and Its Characteristics

Normal spinel LiMn2O4 was synthesized by sol-gel method using lithium nitrate,manganese nitrate,citric acid and ethylene glycol as raw materials.LiMn2O4 was characterized by XRD,TG-DTA,IR,SEMand AAS,The optimum conditions for the synthesis were explored.Citric and ethylene glycol were mixed with molar ratio of 0.25,and the mixtrue was esterified at 140℃ for 4 hours.Then lithium nitrate and manganese nitrate were added with molar ratio of 0.6,In the system,the total molar of cations was equal to that of citric acid.At last,reflux the system at 105℃ for 2 hours,Dried gel was fired at 600℃ for 8 hours.Particle diameters of raw product were about 100nm mainly.Further research shows that lithium ion of LiMn2O4 is easy to be extracted,and normal spinel λ-MnO2 can be obtained after lithium ion extraction.     

Al2O3-SiO2-ZrO2-TiO2复合薄膜结构及形貌的研究

以Al(NO3)3.9H2O、Si(OC2H5)4、ZrOCl2.8H2O和Ti(OC4H9)4为原料,用sol-gel法通过分步水解得到透明稳定性能好的复合溶胶,利用浸渍提拉方法在孔隙率为45%的-αAl2O3陶瓷基体表面涂覆凝胶膜经热处理得到陶瓷膜。采用XRD、FT-IR和SEM测试技术对膜的相组成、凝胶膜热处理中的变化和复合膜的微观形貌进行表征。结果表明,改变Ti组分的加入量,复合膜的主晶相将发生改变;提高热处理温度,胶体颗粒之间将生成更加稳定致密的氧桥键Si—O—Al和Ti—O—Al—O—Si等,从而提高薄膜的机械强度;适中的溶胶粘度是成膜的关键因素。     

纳米钕基氧化物的溶胶-凝胶法制备及其催化性能

采用乙二醇溶胶-凝胶法制备氧化钕基氧化物纳米粒子,研究乙二醇与Nd3+的摩尔比、煅烧温度和掺杂对产物结构的影响及其对高氯酸铵热分解的催化性能。研究表明:当乙二醇与Nd3+的摩尔比为10,70℃加热回流2 h,90℃干燥26 h,700℃煅烧2 h,可得到平均粒径为43.6 nm的球形纳米氧化钕;3.4 mol%Mn掺杂Nd2O3纳米粉体催化高氯酸铵热分解使其在310~350℃和400~470℃的2个小放热峰合并为一个以347.7℃为中心的强放热峰,表观分解热由515 J/g上升到1 250 J/g,高于纳米Nd2O3催化下的1140 J/g,证明了Mn2+掺杂可进一步提高纳米Nd2O3的催化活性。更多还原     

Na2O-B2O3-SiO2系统玻璃结构驰豫的研究

采用正硅酸乙酯、硼酸、乙醇钠作为先驱体,采用的先驱体溶剂分别为乙醇、乙二醇甲醚和乙醇。用热饱和方法对样品进行处理制备大块干胶和玻璃,将处理好的凝胶玻璃进行膨胀系数曲线的测定。实验结果表明,用Sol-gel法制备的Na2O-B2O3-SiO2系统玻璃类似于熔制法得到的淬火玻璃的结构特性,内部质点无充分驰豫的条件。膨胀系数曲线为典型的熔制法淬火玻璃膨胀系数曲线。试样经过反复测试后,凝胶玻璃的膨胀系数曲线与经过退火玻璃的曲线一致。     

中孔Co_3O_4材料的电容特性

采用"原位合成模板法"以硅酸为模板、硝酸钴为钴源,制备了中孔Co3O4材料,研究了模板和硝酸钴的质量比对所制得的中孔Co3O4材料的微观结构和电化学性能的影响.用N2等温吸附—脱附和X线衍射测试了其微观结构.结果表明,随着模板质量比的增加,制备得到的Co3O4材料的比表面积增加,中孔结构越明显,结晶性逐渐降低.在6 mol/L氢氧化钾电解液中测试了其电化学性能,最优质量比制得的样品在5 mV/s扫描速率下的比电容达329 F/g.即使在较高扫描速率下,该质量比的中孔Co3O4比电容依然具有很好的保持性.     

Upeonversion Luminescence of Er3＋, Tin3＋ and Yb3＋ Co-doped Gd3Ga5O12 Nanocrystals

A series of Er3+,Tm3+ and Yb3+ doped Gd3Ga5O12 nanocrystals were prepared by a combustion method.The X-ray diffraction(XRD),field emission scanning electron microscope(FESEM)and upconversion(UC)emission spectra were used to characterize the samples.The results of XRD indicate that Gd3Ga5O12:Er3+,Tm3+,Yb3+ nanocrystals with cubic phase can be obtained.Under the excitation of a 980 nm laser,the different rare earth ions doped Gd3Ga5O12 nanocrystals show upconversion luminescence involving the green emission attributed to the 2H11/2→4I15/2,4S3/2→4I15/2 transitions of Er3+ ions,respectively,the red emissions assigned to the 4F9/2→4I15/2 transitions of Er3+ ions and the 1G4→3F4 as well as 3F2,3→3H6 transitions of Tm3+ ions,respectively,the blue emission attributed to 1G4→3H6 transitions of Tm3+ions,and the near-infrared assigned to the 3H4→3H6 transitions of Tm3+ ions.The CIE coordinates for the samples are calculated.The dependence of their upconversion luminescence properties on Yb3+ ion concentration is investigated.