低温固相反应法制备的NiFe2O4纳米颗粒的结构与磁性

采用低温固相反应法制备了晶粒尺寸在8-47 nm之间的NiFe2O4纳米颗粒系列样品,用X射线衍射仪(XRD)、高分辨中子粉末衍射谱仪、振动样品磁强计和超导量子干涉仪等对样品的晶体结构、宏观磁性和纳米颗粒的表面各向异性进行了分析研究.XRD和中子衍射测量结果显示纳米颗粒的晶格常数略高于块体材料,样品的氧参量表明纳米颗粒的晶格畸变程度没有块体材料严重.相对块体材料,纳米颗粒具有较小的磁化强度、较大的矫顽力和各向异性能密度.纳米颗粒从多畴转变为单畴的临界尺寸约为40 nm,超顺磁性临界尺寸约为16 nm.     

退火温度对ZrO2纳米材料中Eu3+离子发光的影响

研究了退火温度对ZrO₂纳米材料中Eu³⁺离子发光性质的影响. 材料的结构、晶粒尺寸和形状以及晶格的排列分别由XRD，TEM表征. 结果表明：用共沉淀法制备的ZrO₂纳米材料具有不随退火温度变化、稳定的四方结构；材料的晶粒尺寸随退火温度的提高而增大；晶格的排列由无序逐渐变为有序；发射光谱表明其主要发射在595 nm和604 nm处；在394 nm的紫外光辐照下得到了不同样品的604 nm荧光发射强度的变化不同. 这种现象与样品中O^2-离子含量和样品表面的表面缺陷有关；另外，电荷迁移带随退火温度的变化而变化.     

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.     

沉积于MgO基片上的La0.7Ca0.3MnO3薄膜的应变弛豫和磁电阻特性

利用90°离轴射频磁控溅射方法将La_0.7Ca_0.3MnO₃(LCMO)沉积于(001)取向的MgO单晶基片上,薄膜厚度变化范围为5nm到200nm. 通过掠入射X射线衍射技术测量了LCMO/MgO薄膜的面内晶格常数, 结合常规X射线衍射研究了LCMO薄膜的晶格应变及其弛豫情况, 用四探针法测量了薄膜的磁电阻特性.结果表明, LCMO/MgO薄膜均为(001)取向生长, 在厚度小于5nm时已经发生应变弛豫, 当薄膜厚度为100nm以上时, 薄膜的微应变接近于完全弛豫, 并表现出与块体材料类似的磁电阻特性, 具有较大的磁电阻和较高的磁电阻峰值温度.     

晶粒尺寸对CoSb3化合物热电性能的影响

系统地研究了晶粒尺寸对CoSb₃化合物热电性能的影响规律，结果表明晶粒尺寸对CoSb₃化合物的晶格热导率κ_p、电导率σ、能隙宽度E_g和Seebeck系数α有显著影响.当晶粒尺寸由微米尺度减小到纳米尺度时，晶格热导率κ_p显著降低，Seebeck系数α有较大幅度的增加，能隙宽度E_g变宽，电导率σ有一定程度的下降.平均晶粒尺寸为200nm的CoSb₃化合物在温度为700K时，ZT值达到0.43，比平均晶粒尺寸为5000nm的试样增加了4倍.     

硼(氮、氟)掺杂对TiO2纳米颗粒光学性能的影响

利用X射线衍射谱、拉曼光谱和紫外-可见光吸收光谱研究了硼(氮、氟)掺杂对TiO₂纳米颗粒光学性能的影响.X射线衍射谱和拉曼光谱结果表明,掺硼(氮、氟)对TiO₂纳米颗粒的锐钛矿相晶体结构无明显影响,而其锐钛矿晶格出现畸变(c/a值增大),这被归因于掺杂原子对TiO₂纳米颗粒表面氧原子缺位沿晶格c轴方向的占据.另外,掺硼(氮、氟)TiO₂纳米颗粒吸收带红移与TiO相似文献   

银催化合成Tb(BO2)3纳米棒

采用固相反应银作催化剂成功合成出棒状结构的稀土硼酸盐Tb(BO₂)₃发光材料. 利用X射线衍射和区域电子衍射研究了产物的结构特性,在700 oC煅烧时,Tb(BO₂)₃纳米棒具有良好晶形. 透射电镜分析表明,Tb(BO₂)₃纳米棒直径为100～200 nm,厚度为30～50 nm,长约3 μm. 基于Ag纳米颗粒附在Tb(BO₂)₃纳米棒的顶端和中部的事实,探讨了Tb(BO₂)₃纳米棒的生长机理. 荧光光谱研究表明,在369 nm紫外光激发下,Tb(BO₂)₃能发出Tb³⁺的特征绿色荧光,发射主峰位于546 nm,归属于⁵D₄→⁷F₅跃迁. 同时,也探讨了煅烧温度对产物的结构、形貌以及发光性质的影响.     

Gd2O3:Eu3+纳米晶的燃烧合成及光致发光性质

采用柠檬酸作燃烧剂用燃烧合成法制备了Gd₂O₃:Eu³⁺纳米晶.用X射线衍射仪(XRD)、高分辨透射电子显微镜(HRTEM)和荧光分光光度计等对Gd₂O₃:Eu³⁺纳米晶的结构、形貌和发光性能进行了分析.结果表明：不同柠檬酸与稀土离子配比(C/M)制备的样品经800℃ 退火1 h后，均得到了纯立方相的Gd₂O₃:Eu³⁺纳米晶，晶粒尺寸约为30 nm，尺寸分布较窄，其中以C/M=1.0时制备的纳米晶结晶性最好，发光强度最大.Gd₂O₃:Eu³⁺纳米晶主发射峰位置均在612 nm处 (⁵D₀→⁷F₂跃迁)，激发光谱中电荷迁移态发生红移，观察到Gd³⁺向Eu³⁺的有效能量传递.对柠檬酸与稀土离子配比(C/M)对结晶度、发光性质等的影响也进行了分析和讨论.     

Co:BaTiO3/Si(100)纳米复合薄膜制备、微结构及其紫外光电子能谱研究

采用脉冲激光气相沉积(PLD)方法，在Si(100)晶面上制备了Co:BaTiO₃纳米复合薄膜.采用X射线衍射(XRD)结合透射电镜(TEM)方法研究了两种厚度Co:BaTiO₃纳米复合薄膜的晶体结构，当薄膜厚度约为30 nm时，薄膜为单一择优取向；当薄膜厚度约为100nm时，薄膜呈多晶结构.原子力显微镜(AFM)分析表明，当膜厚为30nm时，薄膜呈现明显的方形晶粒.采用紫外光电子能谱(UPS)研究了Co的价态和Co:BaTiO₃纳米复合薄     

海藻酸改性的空心Fe3O4纳米颗粒的制备与应用

不使用任何模板一步制得空心Fe₃O₄纳米颗粒,然后将海藻酸钠嫁接在氨基化的空心Fe₃O₄表面,再利用海藻酸盐与钙离子的作用,在空心Fe₃O₄表面形成一个凝胶化层,制得海藻酸盐凝胶化的空心Fe₃O₄纳米颗粒,粒径约为400～500 nm．采用TEM、XRD、XPS、VSM等手段对纳米微球进行表征．VSM表征结果表明在室温下样品磁性材料为超顺磁性．改性Fe₃O₄纳米颗粒成功地用于柔红霉素的载负和缓释,最大载负率和载药量分别为28.4%和14.2%．缓释结果表明,海藻酸盐凝胶化层的存在,能更有效控制柔红霉素缓慢地释放．     

Temperature dependence of magnetic properties of NiFe2O4 nanoparticles embeded in SiO2 matrix

Spinel ferrite NiFe₂O₄ nanoparticles (?25 nm) in SiO₂ matrix were prepared by sol–gel method. The phase and average crystallite size of the samples were determined by X-ray diffraction method and the particle size distributions were studied by a transmission electron microscope. Magnetic properties of the samples were investigated with different ferrite particle sizes and at various temperatures down to 10 K. Superparamagnetic properties were observed at room temperature when the particle size is less than 10 nm.In superparamagnetic state, the field dependence of magnetization follows Langevin function which was originally developed for paramagnetism. The effective anisotropy constant K_eff is found to increase significantly with the decrease in particle volume and an order of magnitude higher than that of the bulk samples when the particle size is below 5 nm due to the dominance of surface anisotropy. In case of nanosized systems, the effect of size reduction on the law of approach to saturation has also been studied in detail.     

Investigation of structural and magnetic properties of Ni, NiFe and NiFe2O4 thin films

Soft magnetic thin films of Ni, NiFe and NiFe₂O₄ were prepared using reactive magnetron sputtering in various deposition conditions. Experimentally observed soft magnetic property was compared and correlated with nanocrystalline structure evolution. Ni and NiFe deposited films are textured with fcc(111) phase preferred orientation. Accordingly, grain size and lattice parameter were calculated from X-ray diffraction (111) peak line width and 2θ peak position. Addition of reactive gas oxygen in deposition process has substantial effect on crystalline structure of film. There is phase transition from the ordered NiFe (111) structure to the NiFe₂O₄ nanocrystalline phase. The resulting film has shown small X-ray diffraction intensity peak corresponding to (311) and (400) orientation, indicating small amount of existing NiFe₂O₄ phase. The mechanism has been discussed to be responsible for nanocrystallization and amorphization of NiFe₂O₄ films. Magnetic measurement (M-H) loop reveal soft magnetic nature of films with magnetic anisotropy. The coercivity (H_c) of films is in accordance with random anisotropy model, where H_c reduced with grain size. The structural transformation was supported by Fourier transforms infrared spectroscopy measurement. The films are highly smooth with surface roughness in the range of ∼0.53-0.93 nm. NiFe₂O₄ films have shown lowest surface roughness with highest electrical resistivity values. The structural, surface, magnetic and infrared spectroscopy results are observed and analyzed.     

The effect of 3-aminopropyltrimethoxysilane on the formation of NiFe2O4/SiO2 nanocomposites

NiFe₂O₄/SiO₂ nanocomposites were prepared using a sol–gel method with the addition of 3-aminopropyltrimethoxysilane (APS). Different phases and morphologies of NiFe₂O₄/SiO₂ nanocomposites were obtained when different amounts of APS were used. The structural properties of the products were examined by X-ray diffraction (XRD) and transmission electron microscopy (TEM). Sheet-like morphology was observed at higher molar ratio of APS to NiFe₂O₄, while spherical NiFe₂O₄/SiO₂ nanoparticles separated from each other were formed at lower molar ratio of APS to NiFe₂O₄. The magnetic properties of the nanocomposites were also investigated, indicating that the interparticle interactions exhibit strong dependence on the molar ratio of APS to NiFe₂O₄.     

Magnetic properties of La-substituted NiFe2O4 via egg-white precursor route

Nano-sized NiFe_2−xLa_xO₄ ferrites (x=0.00, 0.01, 0.02, 0.03, 0.04, 0.5, 0.07 and 0.09) were synthesized for the first time by using metal nitrate and egg-white extract in aqueous medium. The ferrites were characterized by DTA-TG, XRD, TEM, FT-IR and VSM techniques. The thermal decomposition behavior revealed that the precursors were completely decomposed at about 420 °C. TEM image shows agglomerated nanoparticles with crystallite sizes agrees well with that estimated by XRD measurement. XRD patterns show a secondary phase of LaFeO₃ besides the cubic structure of the La-substituted ferrites. The lattice parameters, X-ray density and crystallite size were found to increase with the increasing La content. The VSM measurement exhibited a ferromagnetic property for all the samples at room temperature. With increasing La, M_s was found to decrease while H_c increased. The decrease in the saturation magnetization is attributed to the paramagnetic properties of lanthanum, which prefer to substitute iron present in the octahedral sites. The increase in the coercivity is due to either the stronger magnetocrystalline anisotropy induced by La substitution or the change in the crystallite size.     

Influence of organic precursor on the structural and magnetic properties of Co3O4 nanoparticles

Antiferromagnetic Co₃O₄ nanoparticles were synthesized by the coprecipitation method. With the addition of the sucrose as chelating agent (sucrose) the size of the particles was reduced from 54 nm to 19 nm. The Co₃O₄ nanoparticles exhibit a cubic spinel structure identified for X-ray diffraction (XRD) and confirmed by Rietveld refinement. Scanning Electron Microscopy (SEM) images exhibit a spherical-like morphology and confirm the decrease of the particle size observed by XRD. The magnetic measurements as a function of temperature using a superconducting quantum interference device (SQUID) show a large surface anisotropy for samples obtained with the addition of sucrose accompanied by an exchange Bias effect indicating also the existence of a weak ferromagnetism. A decrease of the Néel temperature from the bulk (and other nanostructures-type) was observed, which can be associated with finite-size effect in the nanoparticles' shape.     

Finite size effects on the structural and magnetic properties of sol–gel synthesized NiFe2O4 powders

Nanoparticles of nickel ferrite have been synthesized by the sol–gel method and the effect of grain size on its structural and magnetic properties have been studied in detail. X-ray diffraction (XRD) studies revealed that all the samples are single phasic possessing the inverse spinel structure. Grain size of the sol–gel synthesized powders has been determined from the XRD data and the strain graph. A grain size of 9 nm was observed for the as prepared powders of NiFe₂O₄ obtained through the sol–gel method. It was also observed that strain was induced during the firing process. Magnetization measurements have been carried out on all the samples prepared in the present series. It was found that the specific magnetization of the nanosized NiFe₂O₄ powders was lower than that of the corresponding coarse-grained counterparts and decreased with a decrease in grain size. The coercivity of the sol–gel synthesized NiFe₂O₄ nanoparticles attained a maximum value when the grain size was 15 nm and then decreased as the grain size was increased further.     

Preparation and Characterization of Polypyrrole/Ferrospinel Nanocomposite by W/O Microemulsion Pathway

A polypyrrole/ferrospinel(NiFe₂O₄) nanocomposite was prepared by the in situ chemical oxidizing of pyrrole in the presence of NiFe₂O₄ nanoparticles in water-in-oil (w/o) microemulsion. The structural, morphological, and magnetic properties of the as-prepared polypyrrole/NiFe₂O₄ nanocomposite were characterized by X-ray diffraction (XRD), Fourier transform infrared spectra, scanning electron microscopy (SEM), transmission electron microscopy (TEM), and magnetic measurements. XRD and FTIR revealed the presence of NiFe₂O₄ in the nanocomposite. SEM and TEM images illustrated that polypyrrole was coated on the NiFe₂O₄ surface. The electromagnetic parameters, such as conductivity, saturation magnetization, and coercivity of NiFe₂O₄ nanoparticles varied after coating with polypyrrole.     

Studies on polyethylene glycol coating on NiFe2O4 nanoparticles for biomedical applications

The NiFe₂O₄ nanoparticles were prepared by the combustion method and these nanoparticles were successfully coated with polyethylene glycol (PEG) for the possible biomedical applications such as magnetic resonance imaging, drug delivery, tissue repair, magnetic fluid hyperthermia etc. The structural and magnetic characterizations of NiFe₂O₄ nanoparticles were carried out by x-ray diffraction and vibrating sample magnetometry techniques, respectively. The morphology of the uncoated and coated nanoparticles was studied by scanning electron microscopy. The existence of PEG layer on NiFe₂O₄ nanoparticles was confirmed by fourier transform infrared spectroscopy technique.     

Magnetic characterization of surface-coated magnetic nanoparticles for biomedical application

The influence of the oleic acid surface coating on Fe₃O₄ and NiFe₂O₄ nanoparticles on their magnetic and calorimetric characterization was investigated. Fe₃O₄ nanoparticles (particle sizes of 15-20 and 20-30 nm) and NiFe₂O₄ nanoparticles (particle sizes of 20-30 nm) were dispersed in oleic acid. The surface coating resulted in a decrease in the dipole-dipole interaction between the particles, which in turn affected the coercivity and heat dissipation of the nanoparticles. The coercivity of the oleic-acid-coated nanoparticles was found to be lower than that of the uncoated nanoparticles. The temperature rise in the oleic-acid-coated nanoparticles was greater than that of the uncoated nanoparticles; this temperature rise was associated with the relaxation losses. The viscosity dependence on the self-heating temperature of Fe₃O₄ nanoparticles (15-20 and 20-30 nm) under an ac magnetic field was measured. The temperature rise for both the Fe₃O₄ nanoparticles (15-20 and 20-30 nm) exhibited a strong dependence on viscosity at each magnetic field frequency, and the contribution of Brownian relaxation loss to the temperature rise was revealed. Moreover, an in vitro cytotoxicity test of Fe₃O₄ and NiFe₂O₄ was performed using human cervical carcinoma cells (HeLa), and the cytotoxicity of NiFe₂O₄ nanoparticles was compared to that of Fe₃O₄ nanoparticles.     

Solid state reaction synthesis of NiFe2O4 nanoparticles

Ni-ferrite (NiFe₂O₄) nanoparticles have been synthesized via a solid state reaction process. Ni and Fe bi-metallic nanoparticles in the form of Ni₃₃Fe₆₇ alloy nanopowder are first synthesized by simultaneous evaporation of the required amounts of pure Ni and Fe metals followed by rapid condensation of the evaporated metal flux into solid state by means of an inert gas, helium, using the process of inert gas condensation (IGC). In order to form the NiFe₂O₄ structure, as-synthesized samples (Ni₃₃Fe₆₇) are annealed for 12 h in ambient conditions at different annealing temperatures. Structural analyses show that NiFe₂O₄ starts to form at around 450 °C and gets progressively well defined with increasing annealing temperatures yielding particle with size ranging between 15 and 50 nm. Besides successfully forming NiFe₂O₄, NiO/Fe₃O₄ core/shell nanoparticles have also been synthesized by adjusting the annealing conditions. Three different structures, Ni₃₃Fe₆₇, NiO/Fe₃O₄, and NiFe₂O₄, obtained in this study are compared with respect to their structural and magnetic properties.