多孔TiO2/Al/SiO2纳米复合结构的紫外光吸收特性研究

在SiO₂玻璃衬底上用脉冲激光沉积(PLD)技术，分别沉积Ti和Ti/Al膜，经电化学阳极氧化成功制备了多孔TiO₂/SiO₂和TiO₂/Al/SiO₂纳米复合结构. 其中TiO₂薄膜上的微孔阵列高度有序，分布均匀. 实验研究了Al过渡层对多孔TiO₂薄膜光吸收特性的影响. 结果表明：无Al过渡层的多孔TiO₂薄膜其紫外吸收峰在27     

焙烧温度对SiO2负载的Co3O4纳米粒子表面氧缺陷浓度和CO氧化催化性能的影响

以传统的浸渍法,在不同焙烧温度下制备了用于CO氧化反应的Co₃O₄/SiO₂催化剂．通过激光拉曼光谱(Raman)、X射线光电子能谱(XPS)、X射线衍射(XRD)、程序升温还原(TPR)和X射线吸收精细结构谱(XAFS)表征了该系列催化剂的结构．在所有的催化剂中,XRD和Raman光谱都只检测到了Co₃O₄晶相的存在．与Co₃O₄体相相比,XPS结果表明在200 oC焙烧的(Co₃O₄(200)/SiO₂)催化剂中Co₃O₄表面上存在着过量的Co²⁺．与XPS的结果一致,TPR结果表明Co₃O₄(200)/SiO₂催化剂中Co₃O₄表面上存在氧缺陷, 并且XAFS结果也表明Co₃O₄(200)/SiO₂催化剂中Co₃O₄具有更多的Co²⁺．提高焙烧温度使得过量的Co²⁺进一步氧化为Co³⁺,同时降低了表面氧缺陷浓度,从而得到计量比的Co₃O₄4/SiO₂催化剂．在所有的负载催化剂中Co₃O₄(200)/SiO₂催化剂表现出了最好的CO氧化催化性能,表明过量Co²⁺和表面氧缺陷的存在能够促进Co₃O₄催化CO氧化反应的活性.     

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.     

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。     

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。     

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.     

层间热处理对SiO2/ZrO2双层膜的影响

 以正硅酸乙酯和丙醇锆为前驱体,用溶胶-凝胶法在K9基片上提拉镀制SiO₂/ZrO₂双层膜。采用不同实验步骤制备了2个样品,样品1镀完SiO₂后直接镀ZrO₂ ,样品2镀完SiO₂经热处理后再镀ZrO₂。采用原子力显微镜、椭偏仪、紫外-可见分光光度计对薄膜进行表征。针对SiO₂/ZrO₂双层膜,考虑到膜间渗透的影响,采用３层Cauchy模型进行椭偏模拟,椭偏参数的模拟值曲线与椭偏仪的测量值曲线十分吻合,进而发现热处理可以使SiO₂/ZrO₂双层膜之间的渗透减少近23 nm,从而提高其峰值透射率。利用输出波长1.064 mm,脉宽8.1 ns的激光束对样品进行了损伤阈值的测试,用光学显微镜观察损伤形貌,结果发现两者损伤阈值分别为13.6 J/c2和14.18 J/cm²,均为膜的本征损伤。     

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,     

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.     

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.     

Structural,magnetic and dielectric properties of (Li1+, Al3+) co-doped Ni0.5Zn0.5Fe2O4 ferrite ceramics prepared by the sol-gel auto-combustion method

(Li¹⁺, Al³⁺) co-doped Ni_0.5Zn_0.5Fe₂O₄ ferrites, Ni_0.5-xZn_0.5-xLi_xAl_xFe₂O₄ (x = 0.000, 0.025, 0.050 and 0.100), were synthesized by the sol-gel auto-combustion method. X-ray diffraction (XRD), field emission scanning electronic microscope (FESEM), vibrating sample magnetometer (VSM) and LCR meter were used to investigate the structural, magnetic and dielectric properties. Results of XRD and SEM indicate that both doping amount and calcination temperature play significant roles in crystal structure and grain growth. Also, it can be observed that the saturation magnetization and the coercivity change in a noticeable manner. The Ni_0.475Zn_0.475Li_0.025Al_0.025Fe₂O₄ ferrite sintered at 1200 °C has a relatively low coercivity value (62.93 Oe) and the largest saturation magnetization (110.95 emu/g). Besides, dielectric behavior is also improved by Li¹⁺ and Al³⁺ co-doping.     

Structural and magnetic properties of sol-gel Co2xNi0.5−x Zn0.5−xFe2O4 thin films

Nanocrystalline Co_2xNi_0.5−xZn_0.5−xFe₂O₄ (x=0−0.5) thin films have been synthesized with various grain sizes by a sol-gel method on polycrystalline silicon substrates. The morphology as well as magnetic and microwave absorption properties of the films calcined at 1073 K were studied using X-ray diffraction, scanning electron microscopy, X-ray photoelectron spectroscopy, and vibrating sample magnetometry. All films were uniform without microcracks. The Co content in the Co-Ni-Zn films resulted in a grain size ranging from 15 to 32 nm while it ranged from 33 to 49 nm in the corresponding powders. Saturation and remnant magnetization increased with increase in grain size, while coercivity demonstrated a drop due to multidomain behavior of crystallites for a given value of x. Saturation magnetization increased and remnant magnetization had a maximum as a function of grain size independent of x. In turn, coercivity increased with x independent of grain size. Complex permittivity of the Co-Ni-Zn ferrite films was measured in the frequency range 2-15 GHz. The highest hysteretic heating rate in the temperature range 315-355 K was observed in CoFe₂O₄. The maximum absorption band shifted from 13 to 11 GHz as cobalt content increased from x=0.1 to 0.2.     

Characterization and magnetic properties of electrospun Co1−x Zn x Fe2O4 nanofibers

By the electrospinning and calcination techniques, we have prepared uniform nanofibers of Co_1−x Zn _x Fe₂O₄ (0.0≤x≤0.5) ferrites with diameters of 110–130 nm. The Co_1−x Zn _x Fe₂O₄ nanofibers are single-phase spinels and the lattice constant with Zn content deviates from the Vegard’s law for these Co_1−x Zn _x Fe₂O₄ nanofibers. The Co_1−x Zn _x Fe₂O₄ nanocrystal grains by which are built nanofibers increase with calcination temperature. Variations of coercivity and saturation magnetization with calcination temperature can be explained in terms of the grain-size (D) effect. The coercivity (H _c) of Co_0.5Zn_0.5Fe₂O₄ nanofibers varies as D ^0.65 and basically follows the predicted D ^2/3 dependence based on the random anisotropy model in a D range below the single-domain size around 40 nm. The saturation magnetization of Co_1−x Zn _x Fe₂O₄ nanofibers initially increases with increasing Zn content, reaches a maximum value at x=0.3 and then decreases with further increase of Zn content, while the coercivity exhibits a continuous reduction with the increase of Zn content.     

Solvothermal one-step synthesis of MWCNTs/Ni0.5Zn0.5Fe2O4 magnetic composites

A magnetic multi-walled carbon nanotubes-based (MWCNTs-based) composite, MWCNTs/Ni_0.5Zn_0.5Fe₂O₄, was synthesized via a facile solvothermal approach. The composites were characterized by X-ray diffraction analysis, transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), and vibrating sample magnetometry. The results confirmed that MWCNTs and Ni_0.5Zn_0.5Fe₂O₄ coexisted in the composites. The TEM and HRTEM results showed a thick layer of Ni_0.5Zn_0.5Fe₂O₄ was intimately connected to the surface of MWCNTs. The saturation magnetization value of the composites was 45.8 emu/g. Furthermore, the probable synthesis mechanism of the magnetic composites was also investigated based on the experimental results.     

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.     

Reentrant spin glass behavior and large initial permeability of Co0.5−xMnxZn0.5Fe2O4

A series of polycrystalline ferrites having nominal chemical composition Co_0.50−xMn_xZn_0.5Fe₂O₄ (0<x<0.4) have been synthesized by the solid-state reaction technique. The XRD analysis confirms single phase cubic spinel structure for all compositions. Lattice constant increases from 0.84195 to 0.84429 nm with the increasing Mn content and obeys Vegard's law. The average grain size increases by increasing both Mn content and sintering temperatures. Room temperature saturation magnetization increases for x=0.1 and decreases for increasing Mn content. The coercivity decreases with increasing Mn content due to the decrease of anisotropy constant. A reentrant spin glass behavior of these samples is observed from the zero field cooled magnetization measurements. The real part of the initial permeability increases by increasing both Mn content and sintering temperatures. This is due to the homogeneous grain growth and densification of the ferrites. The highest initial permeability 137 is observed for x=0.4 sintered at 1573 K on the other hand, the highest relative quality factor (2522) is obtained for the sample Co_0.2Mn_0.3Zn_0.5Fe₂O₄ sintered at 1523 K. The Mn substituted Co_0.50−xMn_xZn_0.5Fe₂O₄ ferrites showed improved magnetic properties.     

Low-temperature synthesis and growth of superparamagnetic Zn0.5Ni0.5Fe2O4 nanosized particles

Mono-disperse spinel Ni_0.5Zn_0.5Fe₂O₄ nanosized particles have been synthesized via a hydrothermal method at low temperature. X-ray diffraction (XRD), transmission electron microscope (TEM) and high-resolution transmission electron microscope (HRTEM) analysis indicated that the synthesized nanocrystals were of pure cubic spinel structure with the size about 6-20 nm. The activation energy of grain growth is 35.06 kJ/mol experimented by the Arrhenius equation. A primary experimental model was put forward to shed light on the growth mechanism of crystallined spinel Ni-Zn ferrite nanosized particles under hydrothermal conditions. The magnetic measurements shows that the prepared Ni_0.5Zn_0.5Fe₂O₄ nanoparticle possess good superparamagnetic behavior.     

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.     

Structure and magnetic properties of Ni0.5Zn0.5Mn0.5-xMoxFe1.5O4 ferrites prepared by sol-gel auto-combustion method

A series of Mo doped Ni-Mn-Zn ferrites compounds with the formula Ni_0.5Zn_0.5Mn_0.5-xMo_xFe_1.5O₄ (x = 0, 0.025, 0.05, 0.075 and 0.1) were first synthesized by sol-gel auto-combustion method. The X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), Fourier transform infrared spectroscopy (FTIR), and vibrating sample magnetometer (VSM) analysis were carried out to characterize the microstructural and magnetic properties of ferrites. Rietveld refinement of X-ray diffraction data confirmed the formation of cubic spinel structure and the emergence of FeMoO₄ phase with the substitution of Mo⁶⁺ contents. The grain size increased remarkably due to the formation of the liquid phase. The saturation magnetization (M_s) increased while the coercivity (H_c) decreased from 67.3 to 12.1 Oe due to the decrease of magneto-crystalline anisotropy constant. The initial permeability (μ_i) increased significantly from 34 (x = 0) to 114 (x = 0.075) and later decreased for x = 0.1. In our experiment, Ni_0.5Zn_0.5Mn_0.425Mo_0.075Fe_1.5O₄ ferrite presented the best microstructure and soft magnetic properties.