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.     

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。     

聚对苯撑/LiNi0.5Fe2O4纳米复合热电材料的制备及其性能研究

本文以流变相反应法原位合成了聚对苯撑/LiNi_0.5Fe₂O₄纳米复合热电材料,并对其热电性能进行表征,研究了放电等离子烧结时保温时间对其热电性能的影响.结果发现,复合材料铁氧体颗粒粒径为100---300nm,其外部被一层聚对苯撑膜包覆.电子在Fe²⁺和Fe³⁺之间的跳跃机理在铁氧体电导中占主导作用,因此聚对苯撑/LiNi_0.5Fe₂O₄复合材料具有n型导电特性.随着保温时间增加,复合材料电导率基本不变,但热导率逐渐增大且Seebeck系数逐渐减小,导致热电优值系数降低.由于结合了有机物高电导率和低热导率以及无机材料高赛贝克系数的优点,所制备的复合材料热电性能较单一材料有较大提高.     

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。     

非晶态SiO2的高温高压转变研究

利用金刚石对顶砧高压装置和激光双面加热技术, 以经700°C热处理后的吉林长白山硅藻土作为非晶态SiO₂样品,在0—4GPa, 1000—1300K温压条件下开展同步辐射X射线衍射原位测试(EDXD方法), 研究非晶态SiO₂在高温高压条件下的结晶转变方式. 测试结果表明, 在0.8—2.4GPa, 1000—1300K温压条件下, 非晶态SiO₂转变成α-石英而非β-石英或方石英, 其结晶温度较常压下非晶态SiO₂晶化所需温度明显较低, 表明压力有利于降低非晶态SiO₂转变的活化能, 并与常压下的结晶产物不同. 在3—4GPa, 1300K温压条件下, 非晶态SiO₂和石英均转变成了柯石英.     

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.     

Sb2Te3 纳米结构的制备与表征

以室温热电性能优异的传统热电材料Sb₂Te₃为研究对象,利用化学气相沉积法制备Sb₂Te₃单晶纳米结构,并研究其生长机理.实验结果表明,不加催化剂时Sb₂Te₃易生长成六方纳米盘,在金催化剂条件下定向生长成纳米线.Sb₂Te₃的形貌与其晶体结构和生长机理有关.Sb₂Te₃为三角结构,Sb和     

SiO2/Si衬底上石墨烯的制备与结构表征

在分子束外延(MBE)设备中,利用直接沉积C原子的方法在覆盖有SiO₂的Si衬底(SiO₂/Si)上生长石墨烯,并通过Raman光谱和近边X射线吸收精细结构谱等实验技术对不同衬底温度(500℃,600℃,700℃,900℃,1100℃,1200℃)生长的薄膜进行结构表征.实验结果表明,在衬底温度较低时生长的薄膜是无定形碳,在衬底温度高于700℃时薄膜具有石墨烯的特征,而且石墨烯的结晶质量随着衬底温度的升高而改善,但过高的衬底温度会使石墨烯质量降低.衬底温度为1100℃时结晶质量最好.衬底温度较低时C原子活性较低,难以形成有序的C-sp²六方环.而衬底温度过高时(1200℃),衬底表面部分SiO₂分解,C原子与表面的Si原子或者O原子结合而阻止石墨烯的形成,并产生表面缺陷导致石墨烯结晶变差.     

静电纺丝法制备Bi2Fe4O9及其磁学性能的研究

采用静电纺丝法合成了纤维状的Bi₂Fe₄O₉前驱体,再对前驱体进行热处理得到了棒状的Bi₂Fe₄O₉.通过X射线衍射、扫描电子显微镜及透射电子显微镜表征了合成样品的物相及形貌特征.结果表明合成的样品为Bi₂Fe₄O₉单相,属于正交晶系;退火处理导致纤维状的前驱体转变为棒状的Bi₂Fe₄O₉.紫外-可见吸收光谱表明制备的Bi₂Fe₄O₉对光的吸收范围广,不仅对紫外光具有较强吸收,而且对可见光也有一定的吸收.通过振动样品磁强计测定Bi₂Fe₄O₉磁滞回线研究其磁学特性,相应的矫顽力H_C≈82 Oe（1 Oe=79.5775 A/m）,剥离顺磁信号后的剩磁M_r≈0.25 emu/g,研究发现Bi₂Fe₄O₉样品具有弱铁磁性,并且软磁性能有所提高.     

SiO2内保护层对LiB3O5晶体倍频增透膜损伤阈值的影响

 利用离子辅助电子束沉积方法在LiB₃O₅基底上镀制了不加SiO₂内保护层和加SiO₂内保护层的倍频增透膜，测量了两类薄膜在波长1 064 nm多脉冲辐照下的激光损伤阈值，获得了两种不同的损伤形貌，并对损伤原因作了初步探讨。实验结果表明：保护层的加入把由基底膜层界面缺陷吸收所决定的阈值改变到由HfO₂膜层内缺陷吸收所决定的阈值，显著提高了倍频增透膜的抗激光损伤能力。     

多孔SiO2包裹磁性纳米颗粒Fe3O4的制备与表征

采用加热分解油酸铁法制备了Fe₃O₄磁性纳米颗粒,并用有机模板和反相微乳液相结合的方法将磁性纳米颗粒包裹在多孔二氧化硅中.用红外光谱(FTIR)研究了不同的处理方式对油酸铁表面官能团的影响及油酸的反应浓度和加热分解油酸铁的过程中升温速率对Fe₃O₄纳米颗粒的影响.结果表明,用乙醇和丙酮处理后的固态蜡状油酸铁表面的油酸基团会受到损害,将不利于加热分解时形成单分散性的Fe₃O₄纳 关键词： 3O₄纳米颗粒')" href="#">Fe₃O₄纳米颗粒 2包裹')" href="#">多孔SiO₂包裹 反相微乳液法 油酸铁     

Ni0.8Zn0.2Fe2O4和CO2Y添加Ni0.8Zn0.2Fe2O4磁性质对比研究

采用固相反应法制备了Ni0.8Zn0.2Fe2O4和2wt％ Co2Y添加Ni0.8Zn0.2Fe2O4铁氧体多晶样品,并对样品的磁性质进行了研究.实验发现,添加Co2Y后,铁氧体的磁损耗明显下降,相同条件下Q值增大到原来的3倍左右.对添加Co2Y引起铁氧体磁损耗下降的原因进行了讨论,认为主要是钴离子掺杂引起的铁氧体磁滞损耗明显降低所导致的.     

Fabrication and magnetic properties of Ni0.50.5Zn0.5Fe2O4 nanofibres by electrospinning

NiZn ferrite/polyvinylpyrrolidone composite fibres were prepared by sol–gel assisted electrospinning.Ni0.5Zn0.5Fe2O4 nanofibres with a pure cubic spinel structure were obtained subsequently by calcination of the composite fibres at high temperatures.This paper investigates the thermal decomposition process,structures and morphologies of the electrospun composite fibres and the calcined Ni0.5Zn0.5Fe2O4 nanofibres at different temperatures by thermogravimetric and differential thermal analysis,x-ray diffraction,Fourier transform infrared spectroscopy and field emission scanning electron microscopy.The magnetic behaviour of the resultant nanofibres was studied by a vibrating sample magnetometer.It is found that the grain sizes of the nanofibres increase significantly and the nanofibre morphology gradually transforms from a porous structure to a necklace-like nanostructure with the increase of calcination temperature.The Ni0.5Zn0.5Fe2O4 nanofibres obtained at 1000 C for 2 h are characterized by a necklace-like morphology and diameters of 100–200 nm.The saturation magnetization of the random Ni0.5Zn0.5Fe2O4 nanofibres increases from 46.5 to 90.2 emu/g when the calcination temperature increases from 450 to 1000 C.The coercivity reaches a maximum value of 11.0 kA/m at a calcination temperature of 600 C.Due to the shape anisotropy,the aligned Ni0.5Zn0.5Fe2O4 nanofibres exhibit an obvious magnetic anisotropy and the ease magnetizing direction is parallel to the nanofibre axis.     

Ag-Au合金/SiO$lt;sub$gt;2$lt;/sub$gt;复合薄膜的制备与表征

以AgNO₃,HAuCl₄和正硅酸乙酯为主要原料,利用溶胶-凝胶法和旋涂技术,通过热处理和紫外光辐射还原得到了不同n_Ag/n_Au（1∶0,2∶1,1∶2,0∶1）的Ag-Au合金/SiO₂复合薄膜.从扫描电子显微镜和X射线衍射谱的结果可以看出得到的薄膜均匀性好,复合薄膜中合金颗粒的尺寸为10 nm左右.利用紫外-可见分光光谱仪研究了复合薄膜的光吸收性能,结果表明,随着n_Ag/n_Au的降低,吸收峰的位置也由最初的Ag纳米粒子的等离子共振吸收峰430 nm附近,逐渐红移到Au纳米粒子的等离子共振吸收峰605和880 nm附近.从光吸收谱可以看出,n_Ag∶n_Au＝2∶1和1∶2的两个样品分别在515,730 nm附近和550,730 nm附近出现表面等离子共振吸收峰.这表明Au-Ag合金固溶体的形成. 关键词： 2')" href="#">Ag-Au合金/SiO₂ 紫外辐射 光吸收性能     

Preparation of Bi2Fe4O9 particles by hydrothermal synthesis and functional properties

In the present study, particles with different Bi₂Fe₄O₉ micro/nanostructures with a few particular morphologies (flower-like nanoplatelets, hierarchical microstructures, perfectly square platelets single crystals, etc.) obtained under specific hydrothermal synthesis conditions were investigated. The role of the processing parameters (such as NaOH concentration, reaction temperature, and reaction duration time) on the phase formation mechanism and on the microstructural characteristics was investigated. All the Bi₂Fe₄O₉ morphologies showed orthorhombic symmetry with space group Pbam. The photocatalytic properties and magnetic behavior as a function of the micro/nanostructural characteristics of various Bi₂Fe₄O₉ powders were determined. In the presence of Bi₂Fe₄O₉, a degradation rate of Rose Bengal in the range of 52–61% was determined after 180?min under UV light irradiation (λ?=?254?nm). Magnetic activity with antiferromagnetic behavior and a transition at ～240?K slightly dependent on the microstructures was found. The role of Bi₂Fe₄O₉ microstructures in the photocatalytic activity and magnetic properties was discussed.     

Structural, magnetic and electrochemical studies on LiCo0.5Fe0.5O2

LiCo_0.5Fe_0.5O₂ was prepared by sol–gel method. The sample had spinel, cubic and hexagonal phases up to 873 K and a single hexagonal phase above 1,073 K. The magnetic properties were studied at room temperature and at 77 K. The large coercivities observed for the samples annealed at 1,073 and 1,273 K show that these samples do not exhibit a simple antiferromagnetic ordering. From the Mössbauer and magnetization measurements, it is concluded that the hexagonal phase is only an antiferromagnet. The above results clearly demonstrate that the simple aqueous-based sol–gel process developed in this work provides a viable method to synthesize the fine cuboidal particles that display discharge capacity as high as ≈165 mAh/g, which is higher than the value obtained by M. Holzapfel et al. (Holzapfel M, Schreiner R, Ott A, Electrochim Acta 46:1063, 2001) for their samples synthesized by using the ion exchange method. This work suggests that the approaches based on solution chemistry are viable processes for synthesizing good quality electrode material.     

Novel one-dimensional polyaniline/Ni0.5Zn0.5Fe2O4 hybrid nanostructure: synthesis,magnetic, and electromagnetic wave absorption properties

For the first time, the novel one-dimensional uniform polyaniline (PANI)/Ni_0.5Zn_0.5Fe₂O₄ (NZFO) hybrid nanorods were synthesized by an in situ polymerization approach with the assistance of ultrasound and magnetic field. Owing to the unique shape, structure, and chemical composition, the as-synthesized hybrid nanorods with different PANI/NZFO mass ratios possess adjustable magnetic properties, high-saturated magnetization, and coercivity. In addition, these hybrid nanorods present stronger reflection loss and a wider absorption band than pure NZFO. Especially, the hybrid nanorods containing 59 wt% NZFO exhibit excellent microwave absorption properties, with a maximum reflection loss (R _L) of ?27.5 dB observed at 6.2 GHz. And the widest absorption band (R _L ≤ ?10 dB) is 8.1 GHz, corresponding to a matching thin thickness of 2 mm. It is superior to the previously reported value of PANI/ferrite. Therefore, these PANI/NZFO hybrid nanorods may be candidates for lightweight, low-cost, broadband, and highly efficient microwave-absorbing materials.     

Preparation and characterization of novel Pd/SiO2 and Ca-Pd/SiO2 egg-shell catalysts with porous hollow silica

Novel egg-shell structured monometallic Pd/SiO₂ and bimetallic Ca-Pd/SiO₂ catalysts were prepared by an impregnation method using porous hollow silica (PHS) as the support and PdCl₂ and Ca(NO₃)₂·4H₂O as the precursors. It was found from transmission electron microscope (TEM), scanning electron microscope (SEM), energy dispersive spectroscopy (EDS) and X-ray diffraction (XRD) that Pd was loaded on PHS with a particle size of 5-12 nm in Pd/SiO₂ samples and the Pd particle size in Ca-Pd/SiO₂ was smaller than that in Pd/SiO₂ since Ca could prevent Pd particles from aggregating. X-ray photoelectron spectroscopy (XPS) analyses exhibited that Pd 3d_5/2 binding energies of Pd/SiO₂ and Ca-Pd/SiO₂ were 0.2 and 0.9 eV lower than that of bulk Pd, respectively, as a result of the shift of the electron cloud from Pd to oxygen in Pd/SiO₂ and to both oxygen and Ca in Ca-Pd/SiO₂. The activity of Ca-Pd/SiO₂ egg-shell catalyst for CO hydrogenation and the selectivity to methanol, with a value of 36.50 mmol_CO mol⁻¹_Pd s⁻¹ and 100%, respectively, were much higher than those of the catalysts prepared with traditional silica gel as the support, owing to the porous core-shell structure of the PHS support.     

过渡金属(Fe,Co,Ni,Zn)掺杂金红石TiO2的电子结构和光学性质

采用基于密度泛函理论的第一性原理方法对未掺杂以及不同浓度过渡金属Fe,Co,Ni,Zn掺杂金红石TiO₂的超晶胞体系进行了几何优化,并讨论了其晶格常数,电子能带结构和光学性质.研究结果表明:掺杂前后的晶格参数与实验值偏差在3.6%以下;适量的过渡金属掺杂不但影响体系能带结构,拓宽光吸收范围,而且扮演着俘获电子的重要角色,有利于光生电子-空穴对的有效分离以及增强光吸收能力;Fe,Co,Ni,Zn最佳理论掺杂体系分别为Ti_0.75Fe_0.25O₂,Ti_0.75Co_0.25O₂,Ti_0.75Ni_0.25O₂,Ti_0.83Zn_0.17O₂;Fe,Co,Ni3d态分裂为t_2g和e_g态,分别贡献于价带高能级和导带低能级部分,促进了电子-空穴对的生成,从而可提高TiO₂的光催化性能;Zn3d态电子成对填满轨道,不易被激发,故光催化活性无明显提高.     

Silicon nanoparticles formation in annealed SiO/SiO2 multilayers

We present a study on amorphous SiO/SiO₂ superlattice performed by grazing-incidence small-angle X-ray scattering (GISAXS). Amorphous SiO/SiO₂ superlattices were prepared by high-vacuum evaporation of 3 nm thin films of SiO and SiO₂ (10 layers each) onto Si(1 0 0) substrate. After the deposition, samples were annealed at 1100 °C for 1 h in vacuum, yielding to Si nanocrystals formation. Using a Guinier approximation, the shape and the size of the crystals were obtained. The size of the growing nanoparticles in the direction perpendicular to the film surface is well controlled by the bilayer thickness. However, their size varies more significantly in the direction parallel to the film surface.