针状纳米MnxNi0.5-xZn0.5Fe2O4的共沉淀法制备及表征

通过在碱液中共沉淀Mn²⁺、Ni²⁺和Fe²⁺后制备了棒状的前躯体,前躯体于不同温度煅烧后制得了Mn_xNi_0:5-xZn_0:5Fe₂O₄棒状体. 利用X射线衍射仪和透射电镜对棒状体的物相、形貌及粒径进行了表征,并利用振动样品磁强计对磁性能进行研究. 结果表明长径比大于15的棒状,随着x值的增加,Mn_xNi_0:5-xZn_0:5Fe₂O₄样品的直径增加,长度下降,长径比变小,当x=0.5时其直径在50 nm左右而长径比减小到7～8. 随着x值的增加,样品的矫顽力先增加后减少,x值达到0.4时样品的矫顽力再次增加,当煅烧温度为600 oC,x=0.5时样品的矫顽力最大为134.3 Oe. 饱和磁化强度随着x值的增加先增加后减少,当煅烧温度为800 oC和x=0.2时达到最大为68.5 Oe.     

超声强化合成MgFe2O4纳米颗粒及其机理研究

用超声水解方法制备MgO纳米颗粒,用化学沉淀法制备α-Fe₂O₃纳米颗粒,将MgO/α-Fe₂O₃混合体常温下超声活化2h,400℃固相合成制备出MgFe₂O₄纳米颗粒.通过X射线衍射和透射电子显微镜测试产品的化学成分、晶体结构和形貌尺寸,分析声化学反应机理及其影响因素.研究结果表明:所制备的MgFe₂O₄为尖晶石铁氧体,颗粒尺寸分布在20-30nm之间,粒度分布均匀;超声空化效应提高了化学反应活性、增加反应物的比表面积和反应物之间的接触面积,促进固相合成反应速度,降低反应温度,实现了一般条件下难以完成的化学反应.     

一维Ni0.5Zn0.5Fe2O4/SiO2复合纳米结构的制备及其磁性能

采用溶胶-凝胶法结合静电纺丝技术制备了Ni_0.5Zn_0.5Fe₂O₄/SiO₂复合纳米纤维.利用热重-差热分析、X射线衍射、场发射扫描电镜、高分辨透射电镜和振动样品磁强计研究了前驱体纤维的热分解及相转化过程以及焙烧温度和SiO₂含量对目标纳米纤维的相组成、微观结构、形貌及磁性能的影响.结果表明,在450 ℃焙烧时,立方尖晶石结构已基本形成.随着焙烧温度由450 ℃升高到100     

压力对纳米CoFe2O4/SiO2复合材料结构的影响

 采用溶胶-凝胶工艺和高温高压实验技术,制备了纳米CoFe₂O₄/SiO₂复合材料。利用X射线衍射仪、扫描电子显微镜和振动样品磁强计,对样品的结构、微观形貌和磁性进行了研究,并对CoFe₂O₄中阳离子的占位情况进行了讨论。结果表明,随着处理压力的升高,样品的晶粒尺寸增大,晶格常数减小,比饱和磁化强度增大。通过计算结果可以推断,压力的升高导致CoFe₂O₄中的部分Fe³⁺从A位移向了B位,而部分Co²⁺则从B位移向了A位。     

纤维状TiO2/Bi2O3光催化剂的制备及其光催化性能

以C₁₆H₃₆O₄Ti和Bi(NO₃)·5H₂O为原料,以棉花纤维为生物模板,合成了系列纤维状TiO₂/Bi₂O₃光催化剂．采用XRD、SEM、UV-Vis等测试技术对样品的相结构、形貌和吸光性能等进行了表征分析．结果表明,样品中的Bi₂O₃为单斜相和四方相共存的混晶,纤维长度达到毫米级,     

块状Ta2O5-TiO2复合气凝胶的制备与表征

 以乙醇钽、钛酸丁酯为原料,以乙醇为溶剂,通过溶胶-凝胶法及超临界干燥成功制备了Ta₂O₅-TiO₂复合气凝胶。用场发射扫描电镜（SEM）、透射电镜（TEM）、扫描电镜模式下的电子能谱仪（EDS）以及比表面积吸附仪（BET）对其进行表征。结果表明:该气凝胶是由粒径在nm量级的Ti和Ta的羟基氧化物胶体颗粒堆积而成的低密度、高比表积的多孔网络结构材料,孔径分布主要集中在5~15 nm,比表面积为492.9 m²/g,密度为90 mg/cm³左右。     

非线性光学晶体HgGa2S4 和 Hg0.5Cd0.5Ga2S4的能带结构、化学键及光学性质研究

用密度泛函理论和非谐振子模型计算了晶体HgGa₂S₄和Hg_0.5Cd_0.5Ga₂S₄的能带结构、态密度、化学成键及线性、非线性光学性质。结果表明：HgGa₂S₄的价带顶部主要是Ga-S成键态的贡献，导带底部主要是Ga-S反键态的贡献; Hg_0.5Cd_0.5Ga₂S₄的价带顶部主要由S-3p轨道组成，导带底部主要是Ga-S反键态的贡献。布居分析表明Ga-S键主要是共价成分，而Hg-S和Cd-S键主要是离子成分。HgGa₂S₄的折射率计算值与实验值在低能量区很好吻合。另外，HgGa₂S₄的能隙计算值比Hg_0.5Cd_0.5Ga₂S₄小，而二阶非线性极化率比Hg_0.5Cd_0.5Ga₂S₄大。     

钴改性Fe3O4-MnO2催化转化生物质合成气制备液体燃料

本文制备了用于费托合成反应的钴改性Fe₃O₄-MnO₂双功能催化剂,并探究了钴负载量对Fe-Co协同效应的影响以及Fe₁Co_xMn₁催化剂的费托合成反应性能. 实验发现,在Fe₃O₄-Mn催化剂中加入Co可促进铁氧化物的还原、增加反应过程中铁位点的活性. 此外,Co的加入可增强Fe-Co金属间的电子转移,加强两者的协同作用,提高催化性能. Co负载较高的Fe₁Co_xMn₁催化剂可进一步促进加氢反应能力,使产品分布向短链烃方向转移. 在280 ^°C、2.0 MPa和3000 h^-1的最佳工况条件下,Fe₁Co₁Mn₁催化剂的液体燃料收率最高.     

Fe3O4/β-CD的高压电学性质研究

 高压下的电学性质测量是获得材料物理性质的有效手段。利用集成在金刚石对顶砧上的薄膜微电路,测量了高压下Fe₃O₄/β-CD（β-糊精）的电导率,并分析了电导率随压力的变化关系。在0～39.9 GPa范围内,Fe₃O₄/β-CD的电导率随压力的增加而逐渐增大,并呈半导体的特征;而在17.0 GPa处其电导率发生突变,表明样品发生了高压相变。在卸压过程中,电导率随压力的变化呈线性关系,并且卸压后样品的电导率不能回到最初的状态,推测这是一个不可逆的高压结构相变。     

电爆炸丝法制备纳米Al2O3粉末

 设计了电爆炸金属丝产生纳米金属氧化物粉末的实验装置，金属丝电爆炸腔采用圆筒结构，纳米粉末经过微孔滤膜过滤收集。成功制备了纳米Al₂O₃粉末，其平均粒度达到64.9 nm。对电爆炸金属丝产生纳米Al₂O₃粉末的物理条件进行了研究。结果表明实验条件对粉末粒度有重要影响：随气压的增加粉末平均粒度变大；随金属丝直径增大粉末平均粒度变大；粉末的平均粒度与电容器的初始储能也有一定的关系。     

Preparation of LiNi0.5Mn0.5O2 cathode materials by urea hydrolysis coprecipitation

Layered LiNi_0.5Mn_0.5O₂ has been successfully synthesized via urea hydrolysis coprecipitation method. Well-crystallized LiNi_0.5Mn_0.5O₂ was obtained after calcinations of coprecipitation precursors and lithium salts at 450 °C for 3 h and following 900 °C for 10 h in air. Both the precursors and LiNi_0.5Mn_0.5O₂ powders show an agglomerated secondary structure with crystalline particles inside. The quasi-spherical morphology of the precursors was maintained during the calcinations. The first charge and discharge capacities of as-prepared LiNi_0.5Mn_0.5O₂ were 200 and 165mAh/g respectively. The discharge capacity of about 160mAh/g was retained after 10cycles for as-prepared samples.     

Synthesis of nanocrystalline Zn0.5Mn0.5Fe2O4 via in situ polymerization technique

Nanocrystalline Zn_0.5Mn_0.5Fe₂O₄ was synthesized through the pyrolysis of polyacrylate salt precursors prepared via in situ polymerization of the metal salts and acrylic acid. The pyrolysis behavior of the polymeric precursors was studied by use of thermal analysis. The as-obtained product was characterized by powder X-ray diffraction (XRD), transmission electron microscope (TEM), electron diffraction (ED) pattern, scanning electron microscopy (SEM) and electron dispersive X-ray (EDX) analysis. The results revealed that the particle size is in the range of 15–25 nm for Zn-Mn ferrites with good crystallinity. Magnetic properties of the sample at 300 K were measured using a vibrating sample magnetometer, which showed that the sample exhibited characteristics of superparamagnetism.     

Effect of calcination temperature on the structure and hydroxylation activity of Ni0.5Cu0.5Fe2O4 nanoparticles

Nanocrystalline Ni_0.5Cu_0.5Fe₂O₄ was synthesized by sol-gel method with varying calcination temperature over the range of 500-1000. The powders obtained were characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). In addition, thermal analysis (TG-DTG-DTA) of the precursor was carried out. The study reveals the simultaneous decomposition and ferritization process at rather low temperature (280-350). For the crystalline structure investigated, single cubic spinel is gained when the precursor was decomposed at 800-1000, whereas separated crystal CuO formed when calcination temperature is below 800. The increase of calcination temperature favors the appearance of Fe_B³⁺, Cu_A²⁺ and O on the spinel surface. The hydroxylation activity is relative to the amount of Cu_B²⁺ species on the spinel surface. The lattice oxygen species on the spinel surface are favorable for the deep oxidation of phenol.     

Effect of sintering temperature and the particle size on the structural and magnetic properties of nanocrystalline Li0.5Fe2.5O4

Sintering temperature and particle size dependent structural and magnetic properties of lithium ferrite (Li_0.5Fe_2.5O₄) were synthesized and sintered at four different temperatures ranging from 875 to 1475 K in the step of 200 K. The sample sintered at 875 K was also treated for four different sintering times ranging from 4 to 16 h. Samples sintered at 1475 K have the cubic spinel structure with a small amount of α-Fe₂O₃ (hematite) and γ-Fe₂O₃ (maghemite). The samples sintered at≤1275 K do not show hematite and maghemite phases and the crystals form the single phase spinel structure with the cation ordering on octahedral sites. Particle size of lithium ferrite is in the range of 13-45 nm, and is depend on the sintering temperature and sintering time. The saturation magnetization increased from 45 to 76 emu/g and coercivity decreases from 151 to 139 Oe with an increase in particle size. Magnetization temperature curve recorded in ZFC and FC modes in an external magnetic field of 100 Oe. Typical blocking effects are observed below about 244 K. The dielectric constant increases with an increase in sintering temperature and particle size.     

Preparation and magnetic properties of BaFe12O19/Ni0.8Zn0.2Fe2O4 nanocomposite ferrite

Nanocomposite of hard (BaFe₁₂O₁₉)/soft ferrite (Ni_0.8Zn_0.2Fe₂O₄) have been prepared by the sol–gel process. The nanocomposite ferrite are formed when the calcining temperature is above 800 °C. It is found that the magnetic properties strongly depend on the presintering treatment and calcining temperature. The “bee waist” type hysteresis loops for samples disappear when the presintering temperature is 400 °C and the calcination temperature reaches 1100 °C owing to the exchange-coupling interaction. The remanence of BaFe₁₂O₁₉/Ni_0.8Zn_0.2Fe₂O₄ nanocomposite ferrite with the mass ratio of 5:1 is higher than a single phase ferrite. The specific saturation magnetization, remanence magnetization and coercivity are 63 emu/g, 36 emu/g and 2750 G, respectively. The exchange-coupling interaction in the BaFe₁₂O₁₉/Ni_0.8Zn_0.2Fe₂O₄ nanocomposite ferrite is discussed.     

低维Bi2Fe4O9晶体的控制生长及其光催化性能研究

Low-dimensional Bi₂Fe₄O₉ nanosheets and microrods have been selectively prepared by a solvothermal method, from which the growth of the Bi₂Fe₄O₉ crystals can be controlled by the variation of reaction conditions. Structure determination showed that the nanosheets are mainly exposed by {001} facets while the microrods are exposed by {110} facets. Ab- sorption spectra revealed that there are two bandgaps observed for both nanosheets (at 1.9 and 1.55 eV) and microrods (1.7 and 1.45 eV), and they both would be available for the sunlight photocatalysis e ciently due to the intensive absorption ability in a wide region. Photocatalytic investigation demonstrated that the overall photocatalytic performance of the microrods is prior to that of the nanosheets due to the variation of bandgaps and exposed facets. The present report provides a useful alternative strategy for the controlling growth of nanostructures and/or microcrystals besides the present demonstration of the Bi₂Fe₄O₉ crystals with diflerent bandgaps and facets that would be able to tune the corresponding photocatalytic ability selectively.     

Flame synthesis of 5 V spinel-LiNi0.5Mn1.5O4 cathode-materials for lithium-ion rechargeable-batteries

The lithium transition metal oxide LiNi_0.5Mn_1.5O₄ with an space group (SG) structure has shown great potential as a cathode material for 5 V lithium-ion rechargeable-batteries. In this work, a flame-assisted spray technology (FAST) was developed to produce nanostructured LiNi_0.5Mn_1.5O₄ powder in a continuous manner. The as-synthesized powder had a uniform morphology, was spherical in shape and had a nanocrystalline structure, as observed by SEM and TEM. The XRD pattern of the as-synthesized powder matched the spectrum of spinel-LiNi_0.5Mn_1.5O₄. The average grain size was about 16 nm, as calculated by XRD. However, XRD also indicated the impurity Mn₂NiO₄ in the powder. By varying flame temperature, it was possible to show that the impurity was formed due to the high temperature of the flame. While flame temperature was minimized by lowering the H₂/N₂ ratio, it was not possible to completely eliminate Mn₂NiO₄ from the as-synthesized powder. After annealing at 800 °C for 2 h, the impurity was eliminated, and the XRD pattern of the powder indicated a pure-phase spinel structure with an SG. The electrochemical performance of the flame-synthesized LiNi_0.5Mn_1.5O₄ powder was tested in coin-type test batteries that were charged and discharged at constant current under a 5 V potential. The test cells showed the characteristic voltage plateaus of spinel-LiNi_0.5Mn_1.5O₄ ( SG). The material proved to be electrochemically active as a cathode material for lithium-ion rechargeable-batteries.     

NbTi0.5Ni0.5O4 as anode compound material for SOFCs

NbTi_0.5Ni_0.5O₄ (NTNO) has been prepared using solid state synthesis and investigated as a potential anode material. The oxide form of NTNO has single phase rutile-type structure with tetragonal (P42/mnm) space group. The reduced form is a composite of nano-scaled particles of metallic Ni and Nb_1.33Ti_0.67O₄ phase. Reduced NTNO showed high electronic conductivity up to 280 S.cm^− 1 at 900 °C in reducing atmosphere, but suffers from low CTE equal to 3.78 10^− 6 K^− 1. Studies of NTNO as anode material were carried out in a three electrode - electrochemical half cell configuration under pure humidified H₂ at 900 °C using a 2 mm thick zirconia electrolyte and without any additional current collector material. The results show a reasonable series resistance (R_s) equal to 2.7 Ωcm² (about 50% higher than for metallic gold layers) indicating a good current collection performance for a 10 μm layer of material. The polarization resistance (R_p) was equal to 33 Ωcm² and is attributed to a poor density of three phase boundaries (TPB) and shortage of oxide ion conduction in the anode layer. The results show the potential of NTNO as an anode material, especially after optimization of the microstructure towards the increase of TPB length.     

Effect of grain size on the magnetic properties of superparamagnetic Ni0.5Zn0.5Fe2O4 nanoparticles by co-precipitation process

Ni_0.5Zn_0.5Fe₂O₄ (NZFO) spinel-type nanoparticles were directly fabricated by the chemical co-precipitation process using metal nitrate and acetate as precursors since nitrogen and carbon would be taken away in the forms of oxynitride and oxycarbide, respectively, after the precursors were annealed and then investigated in detail by employing X-ray diffraction (XRD), magnetic measurement and Raman spectroscopy. XRD analysis indicates that the as-prepared nanocrystals are all of a pure cubic spinel structure with their sizes ranging from 20.8 to 53.3 nm, as well as peaks of some samples shifting to lower angles due to lattice expansion. Calculations from the derived XRD data indicate that the activation energy is 30.83 kJ/mol. The magnetic measurements show that these samples are superparamagnetic. The saturation magnetization increases with annealing temperature, which may be explained by super-exchange interactions of Fe ions occurring at A- and B-sites. The variation of coercivity with particle size is interpreted on the basis of domain structure and crystal anisotropy. Furthermore, these nanoparticles exhibit a redshift phenomenon at lower temperatures seen in the Raman spectra, which could be related to ionic substitution.