Microwave synthesis and characterization of Co-ferrite nanoparticles

Stable CoFe(2)O(4) nanoparticles have been obtained by co-precipitation using a microwave heating system. Transmission electron microscopy images analysis shows an agglomeration of particles with an average size of about 5 nm, and X-ray diffraction reveals the presence of a pure ferrite nanocrystalline phase. X-ray photoelectron spectroscopy and thermal gravimetric analysis show the presence of organic matter in the range of about 16 wt%. The magnetic response in DC fields is typical for an assembly of single-domain particles. The measured saturation magnetization is slightly larger than the bulk value, probably due to the presence of small amounts of Co and Fe. AC magnetization data indicate the presence of magnetic interactions between the nanoparticles.     

ZnFe2O4纳米材料的制备及其顺磁特性研究

采用改进的共沉淀法制备了不同粒径的ＺｎＦｅ２Ｏ３纳米晶体，利用ＸＲＤ和ＴＥＭ技术对其晶体结构和表面形貌进行了研究，结果表明，ＺｎＦｅ２Ｏ４纳米晶体可以在较低的温度下形成，经具有晶粒细小，晶粒大小均匀等优点，用ＥＰＲ技术对其顺磁共振特性进行了研究，探讨了顺磁共振特性变化规律。     

A general, one-step and template-free synthesis of sphere-like zinc ferrite nanostructures with enhanced photocatalytic activity for dye degradation

Spinel zinc ferrite nanospheres with diameters of about 212 nm were synthesized in high yield via a general, one-step and template-free solvothermal route. The prepared nanospheres had cubic spinel structure and exhibited good size uniformity and regularity. The absorption edge of ZnFe(2)O(4) nanospheres shifted to a higher energy in the UV-Vis absorption spectrum compared with that of ZnFe(2)O(4) nanoparticles. The ZnFe(2)O(4) nanospheres exhibited remarkably high surface photovoltage response in the UV and visible region, suggesting the enhanced separation ability of photogenerated electrons and holes. The dramatically enhanced photocatalytic activity of the ZnFe(2)O(4) nanospheres was evaluated in the decomposition of rhodamine B under Xe lamp irradiation. Hydroxyl radicals on the surface of photoilluminated ZnFe(2)O(4) nanospheres were detected by the photoluminescence technique, which suggested that hydroxyl radicals played an important role in the photocatalytic reaction. This study provided new insight into the design and preparation of functional nanomaterials with sphere structure in high yield, and the as-grown architectures demonstrated an excellent ability to remove organic pollutants in wastewater.     

ZnFe2O4中阳离子分布对苯酚H2O2羟化制苯二酚催化活性的影响

具有尖晶石结构的铁酸盐是苯酚H2O2羟化合成苯二酚的有效催化剂.分别用共沉淀和水热法制备了ZnFe2O4,并用Mossbauer,XRD和ESR等方法予以表征.发现不同方法制备的ZnFe2O4中阳离子在四面体和八面体位置的分布不同,认为阳离子分布影响了催化活性.     

静电纺丝法制备铁酸锌中空纤维及其磁学性能

以锌盐、铁盐和聚乙烯吡咯烷酮(PVP)为原料,通过静电纺丝法先制备PVP/硝酸盐复合纤维,这些复合纤维以5℃·min-1的升温速率加热到500℃并保温3h,最终得到铁酸锌(ZnFe2O4)中空纤维.通过X射线衍射(XRD)、扫描电镜(SEM)、透射电镜(TEM)以及振动样品磁强计(VSM)等分析手段对中空纤维的晶体结构、形貌和磁学性能进行了研究.结果显示,ZnFe2O4中空纤维属于尖晶石结构,高温处理后仍能保持一维结构,纤维直径在200-400nm之间,纤维壁由大小为25nm的颗粒堆积而成.室温磁化结果显示制备的ZnFe2O4中空纤维具有超顺磁性,在10kOe的磁化强度为2.03emu·g-1.     

Spin-canting and magnetic anisotropy in ultrasmall CoFe2O4 nanoparticles

The magnetic properties of cobalt ferrite nanoparticles dispersed in a silica matrix in samples with different concentrations (5 and 10 wt% CoFe2O 4) and same particle size (3 nm) were studied by magnetization, DC and AC susceptibility, and Mossbauer spectroscopy measurements. The results indicate that the particles are very weakly interacting. The magnetic properties (saturation magnetization, anisotropy constant, and spin-canting) are discussed in relation to the cation distribution.     

Reduced graphene oxide/ZnFe2O4 nanocomposite as an efficient catalyst for the photocatalytic degradation of methylene blue dye

Research on Chemical Intermediates - This research effort reports the design and development of reduced graphene oxide/zinc ferrite (rGO/ZnFe2O4) nanocomposites for the photo-oxidative degradation...     

Time-resolved spectroscopic behavior of Fe2O3 and ZnFe2O4 nanocrystals

Using nanosecond (ns) and femtosecond (fs) time-resolved absorption spectroscopies (pump-probe technique), the carrier dynamics in transition metal oxide nanocrystals of alpha-Fe2O3 and ZnFe2O4 was studied during the photolysis process. For Fe2O3 and ZnFe2O4 nanocrystals, the fs measurements detect similar profiles of a positive nonlinear absorption in their capped nanocrystals, whereas much weak signals in the naked particles. In the nanosecond measurements Fe2O3 and ZnFe2O4 nanocrystals show obvious excitation-power dependent absorption properties and at the low pump power they show weak photobleaching, but at high pump power they produce positive nonlinear absorptions. For Fe2O3 nanocrystals, the threshold power of negative absorption (bleach) to positive absorption increases with reducing size, whereas for the ZnFe2O4 samples, the threshold powers reach minimum at a critical size of 11 nm, grow for both the bigger and the smaller nanocrystals. These results reflect the influences of their microscopic magnetic couplings and carrier correlation on biexciton absorption in Fe2O3 and ZnFe2O4 nanocrystals. All the results indicate that the time resolved photoabsorption techniques are useful to study the microscopic spin interactions and carrier correlations in transition metal oxide nanocrystals.     

石墨烯/锌铁氧体复合物的制备及抗菌性能

用氧化还原法和化学共沉淀法分别制备了石墨烯(GE)和石墨烯/锌铁氧体(GE/ZnFe2O4)复合物,通过现代测试技术表征了样品的物相结构、组成和微观形貌.以大肠杆菌、金黄色葡萄球菌和白色念珠菌为测试菌种,分别对样品的抗菌性能进行了研究.结果表明,样品的抗菌活性受GE/ZnFe2O4复合物中GE和ZnFe2O4质量比(mG/Z)以及菌种的影响,其中mG/Z=0.4的复合物对三种菌均有较好的抗菌效果,其最小抑菌浓度分别为25、25和12.5μg/mL;复合物对白色念珠菌的抗菌效果最好,这与菌种的结构有关.此外,对样品的抗菌机理进行了详细研究.     

Novel preparation and properties of magnesioferrite nanoparticles

Nano-magnetic magnesium ferrite particles were synthesized by a simple and cost-effective method using different ratios between Mg/Fe precursors and fuel. Significant effects of these ratios on the crystalline phases, crystallite size, particle size, lattice constant, morphological and magnetic properties of the as-synthesized nano-particles have been investigated. Phase evolution, morphological and magnetic characteristics were determined by XRD, SEM, EDX and VSM techniques. The results obtained revealed that the as-prepared Mg ferrite nano-particles have the nanometer size and partially inverse spinel structure. Nano-structured magnesium ferrite spinel has been synthesized with various cyrystallite sizes ranging from 8 to 66 nm. Room temperature magnetization results showed that the magnetic properties of Mg ferrite nano-particles depend upon their size and crystallinity. The saturation magnetization for the sample having the highest crystallite size was 32.85 emu/g.     

尖晶石结构MFe2O4(M=Ca,Mg,Cu,Zn)纳米晶粉末的制备和磁性能

采用新型氨基凝胶自燃法成功制备出尖晶石结构MFe₂O₄（M=Ca,Mg,Cu,Zn）纳米晶粉末。对合成粉体样品的物相、形貌和磁性能进行了详细的研究。经能量色散X射线谱分析确定了合成MFe₂O₄粉末的高纯度。系统地研究了所合成的MFe₂O₄纳米晶粉末的磁性能。所有样品的磁滞回线均较窄,表明了它们具有软磁的特征。经测试得出4种铁氧体的饱和磁化强度（M_s）分别为2.1,29.3,24.1和4.2 emu·g^-1;剩余磁化强度（M_r）分别为0.2,2.3,11.4和0.2 emu·g^-1。这4种铁氧体样品的M_r/M_s值均小于0.5。对CaFe₂O₄和MgFe₂O₄两种典型铁氧体的零场冷却和场冷磁性能作了详细的研究。其中CaFe₂O₄样品的磁化强度在75 K以下有不一致的变化趋势,这是由于其发生了磁相变。     

Ordered mesoporous MFe(2)O(4) (M = Co, Cu, Mg, Ni, Zn) thin films with nanocrystalline walls, uniform 16 nm diameter pores and high thermal stability: template-directed synthesis and characterization of redox active trevorite

In this paper, we report on ordered mesoporous NiFe(2)O(4) thin films synthesized via co-assembly of hydrated ferric nitrate and nickel chloride with an amphiphilic diblock copolymer, referred to as KLE. We establish that the NiFe(2)O(4) samples are highly crystalline after calcination at 600 °C, and that the conversion of the amorphous inorganic framework comes at little cost to the ordering of the high quality cubic network of pores averaging 16 nm in diameter. We further show that the synthesis method employed in this work can be readily extended to other ferrites, such as CoFe(2)O(4), CuFe(2)O(4), MgFe(2)O(4), and ZnFe(2)O(4), which could pave the way for innovative device design. While this article focuses on the self-assembly and characterization of these materials using various state-of-the-art techniques, including electron microscopy, grazing incidence small-angle X-ray scattering (GISAXS), time-of-flight secondary ion mass spectrometry (TOF-SIMS), X-ray photoelectron spectroscopy (XPS), as well as UV-vis and Raman spectroscopy, we also examine the electrochemical properties and show the benefits of combining a continuous mesoporosity with nanocrystalline films. KLE-templated NiFe(2)O(4) electrodes exhibit reasonable levels of lithium ion storage at short charging times which stem from facile pseudocapacitance.     

硬脂酸前驱体法制铁酸锌脱硫剂及其在中温下的应用

以硬脂酸为凝胶剂，经由溶胶、凝胶、煅烧等步骤直接合成了晶体尺寸为纳米级(15nm～32nm)的铁酸锌脱硫剂，并应用TG-DTA、XRD、BET等测试手段对干凝胶及所得产品进行分析表征。结果表明，硬脂酸前驱体法合成温度低，操作简便。随着煅烧温度的升高，产品的比表面积减小，平均粒径增大，脱硫性能变差；该法制备的脱硫剂在350℃~550℃活性高，脱硫精度高，硫容大，而且再生性能良好，450℃下完全再生。     

热处理条件对BaSm0.3Fe11.7O19铁氧体纤维结构演化和磁性能的影响

以金属盐和柠檬酸为原料,采用溶胶凝胶法成功制备1μm以下具有较大长径比的纳米晶BaSm0.3Fe11.7O19 铁氧体纤维。采用热重-差热分析(TG-DSC)、X射线衍射仪(XRD)、场发射扫描电镜(FE-SEM)和振动样品磁强计(VSM)对前躯体纤维及其焙烧产物进行了表征。实验结果表明,750℃焙烧1小时,BaSm0.3Fe11.7O19铁氧体相已基本形成,随着焙烧温度的升高和保温时间的延长,BaSm0.3Fe11.7O19晶粒尺寸逐渐增大,纤维表面越发粗糙,片状结构越发明显。同时,纤维的饱和磁化强度(Ms)随晶粒尺寸的增加而增大,而矫顽力(Hc)则呈现先增大后减小的趋势,在晶粒尺寸为58.4 nm附近达到最大值459.2 kA/m,这表明Sm0.3Fe11.7O19纤维的临界单畴尺寸在60nm左右。对低温(77K)和室温(300K)样品的磁性能比较发现,磁性能存在明显的差异,这主要与纳米晶的表面自旋有关。     

Optimization of catalytic, surface and magnetic properties of nanocrystalline manganese ferrite

Single-domain manganese ferrite nanoparticles have been synthesized with narrow particle size distribution using the combustion technique. Influence of fuel ratios on the as-prepared powders were characterized by XRD, SEM, VSM, N₂ adsorption at −196 °C and conversion of cyclohexene at 200–400 °C. Ratios of fuel to cations were maintained variously at 0.0, 0.67, 1.33 and 2.67.The fuel to cations ratio of 2.67 gives better yield in the formation of nanocrystalline Mn ferrite and single-domain particles with a narrow range of size distribution. Maximum magnetization and coercivity values of the investigated ferrite are also greater for the ratio of 2.67. These values measured at room temperature are found to be 68.58 emu/g and 62.57 Oe, respectively. The BET surface area of the investigated solids was found to decrease by increasing the ratio between fuel and cations due to increasing the flame temperature. However, this treatment resulted in a significant increase in catalytic activity of the as-synthesized solids. All solids investigated behaved as dehydrogenation catalysts. The change in fuel/cations ratios did not alter the mechanism of dehydrogenation of cyclohexene, but increased the concentration of active sites involved in the catalyzed reaction.     

Zn对沉淀铁催化剂结构及其F-T合成性能的影响

采用低温N₂吸附、XRD、MES、CO-TPR和H₂-DTG研究了Zn(100 gFe/x gZn, x=7～100)助剂对 Fischer-Tropsch (F-T) 合成Fe基催化剂的织构性质、还原行为以及相变结构的影响;在H₂/CO=2.0、260 ℃、1.5 MPa和4000 mL/(g·h) 条件下在固定床反应器上考察了Zn助剂含量对Fe基催化剂F-T合成反应活性、烃产物选择性和运行稳定性的影响。研究结果表明,随着Zn含量的增加,氧化态催化剂的物相由α-Fe₂O₃和ZnFe₂O₄逐渐向ZnFe₂O₄和ZnO转变,ZnFe₂O₄在催化剂中优先生成,只有在超出其计量比1∶2之后才有ZnO出现。由于ZnFe₂O₄较为稳定,能够促进催化剂中Fe物相的分散,导致比表面积增加。在还原和反应态催化剂中,ZnFe₂O₄一方面抑制催化剂的过度还原和碳化;另一方面表现为稳定活性相铁碳化物。催化剂的F-T反应性能评价结果表明,纯铁催化剂由于铁碳化物氧化而迅速失活,而Zn助剂催化剂却由于ZnFe₂O₄的稳定作用,活性较为稳定。同时,由于催化剂在反应初相变的影响,导致Zn助剂催化剂的初始烯烃选择性随着Zn含量的增加而增加,在相态稳定之后选择性趋于一致。     

Low temperature synthesis of zinc ferrite nanoparticles

Zinc ferrite (ZnFe₂O₄) nanocrystalline powder materials with various particle sizes were prepared by a unique solid-state combustion method. Phase purity of ZnFe₂O₄ was confirmed by X-ray diffraction studies. High resolution transmission electron microscopic analysis and selected area diffraction pattern also confirmed the correct crystalline phase formation. Particle size was determined from both the transmission electron microscopic images and also from the XRD peak broadening analysis. Oxidation states of different elements present in ZnFe₂O₄ were determined by X-ray photoelectron spectroscopy. Frequency dependent dielectric constant and a.c. conductivity were measured as a function of particle size and both of them were found to decrease with decreasing particle size. These studies indicated that good quality zinc ferrite nanocrystalline powdered materials can be synthesized at low temperature.     

Ultrasmall water-soluble metal-iron oxide nanoparticles as T1-weighted contrast agents for magnetic resonance imaging

Using an improved hydrolysis method of inorganic salts assisted with water-bath incubation, ultrasmall water-soluble metal-iron oxide nanoparticles (including Fe(3)O(4), ZnFe(2)O(4) and NiFe(2)O(4) nanoparticles) were synthesized in aqueous solutions, which were used as T(1)-weighted contrast agents for magnetic resonance imaging (MRI). The morphology, structure, MRI relaxation properties and cytotoxicity of the as-prepared metal-iron oxide nanoparticles were characterized, respectively. The results showed that the average sizes of nanoparticles were about 4 nm, 4 nm and 5 nm for Fe(3)O(4), ZnFe(2)O(4) and NiFe(2)O(4) nanoparticles, respectively. Moreover, the nanoparticles have good water dispersibility and low cytotoxicity. The MRI test showed the strong T(1)-weighted, but the weak T(2)-weighted MRI performance of metal-iron oxide nanoparticles. The high T(1)-weighted MRI performance can be attributed to the ultrasmall size of metal-iron oxide nanoparticles. Therefore, the as-prepared metal-iron oxide nanoparticles with good water dispersibility and ultrasmall size can have potential applications as T(1)-weighted contrast agent materials for MRI.     

Nanophase cobalt, nickel and zinc ferrites: synchrotron XAS study on the crystallite size dependence of metal distribution

Nanophase cobalt, nickel and zinc ferrites, in which the crystallites are in the size range 4-25 nm, were synthesised by coprecipitation and subsequent annealing. X-Ray absorption spectroscopy using synchrotron radiation (supported by X-ray powder diffraction) was used to study the effects of particle size on the distributions of the metal atoms over the tetrahedral and octahedral sites of the spinel structure. Deviations from the bulk structure were found which are attributed to the significant influence of the surface on very small particles. Like the bulk material, nickel ferrite is an inverse spinel in the nanoregime, although the population of metals on the octahedral sites increases with decreasing particle size. Cobalt ferrite and zinc ferrite take the inverse and normal forms of the spinel structure respectively, but within the nanoregime both systems show similar trends in being partially inverted. Further, in zinc ferrite, unlike the normal bulk structure, the nanophase system involves mixed coordinations of zinc(ii) and iron(iii) consistent with increasing partial inversion with size.     

X型六角晶系钡铁氧体纳米晶的制备和表征

用硬脂酸凝胶法制备了Co₂-X型六角晶系钡铁氧体纳米晶,在750℃热处理得到的纳米晶形貌为球形,粒径范围为15～25nm.随着热处理温度的升高,粒子逐渐长大并呈块状.振荡样品磁强计测试结果表明,Co₂-X型六角晶系钡铁氧体纳米晶具有与常规体材料不同的磁性能,其比饱和磁化强度σ_s低于后者.产物的矫顽力、比饱和磁化强度随粒子的长大呈规律性的变化.