Sol-gel synthesis of Bi3.25La0.75Ti3O12 nanotubes

Ferroelectric Bi_3.25La_0.75Ti₃O₁₂ (BLT) nanotubes were synthesized by sol-gel technique using nanochannel porous anodic aluminum oxide (AAO) templates, and were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM) and high resolution transmission electron microscopy (HRTEM). BLT nanotubes with diameter of around 240 nm and the wall thickness of about 25 nm exhibited a single orthorhombic perovskite structure and highly preferential crystal growth along the [1 1 7] orientation, which have smooth wall morphologies and well-defined diameters corresponding to the diameter of the applied template. The formation mechanism of BLT nanotubes was discussed.     

Hydrothermal growth and characterization of magnetite (Fe3O4) thin films

Well-crystallized magnetite (Fe₃O₄) thin films were successfully prepared by a simple hydrothermal process using hydrazine hydrate as the mineralizer. X-ray diffraction and scanning electron microscopy (SEM) and transmission electron microscopy were employed to characterize the products. SEM images show that the uniform Fe₃O₄ film (∼ 3 μm in thickness) is firmly grown on a nickel substrate. The magnetic property of the Fe₃O₄ particles scraped from the film was measured by Physical Property Measurement System (PPMS) at room temperature, and the magnetization curve reveals a soft ferromagnetic behavior with high saturation magnetization of 85 emu/g. Furthermore, the chemical and growth mechanisms for the hydrothermal formation of the Fe₃O₄ film are discussed.     

One-step solvothermal approach for preparing soft magnetic hydrophilic PFR coated Fe3O4 nanocrystals

The hydrophilic phenol formaldehyde resin coated Fe₃O₄ nanocrystals are prepared via a novel one-step solvothermal approach at 160 °C for 6-9 h without inert gas protection. Water-glycol mixture is used as solvent in common air surrounding. FeSO₄·7H₂O, hexamethylenetetramine and phenol are used as resource materials without any others additives or surfactants. The transmission electronic microscope images show the samples are composed of sphere-like particles with sizes about 10-20 nm. The X-ray diffraction data indicate cube-phase Fe₃O₄ nanocrystals are obtained at given conditions. Fourier transform infrared spectra further reveal the samples are consisted of Fe₃O₄ and PFR. Without modified pH and added surfactants, the solubility of the obtained sample is over 1% in water, which is far more than its solubility in toluene. Room-temperature hysteresis loop indicate that the as-obtained nano-crystals possess soft magnetic properties with high saturated mass magnetization (50.6 emu/g) and negligible coercivity.     

Hydrothermal synthesis of YBO3:Tb microflowers and their luminescence properties

Three-dimensional flowerlike YBO₃:Tb³⁺ phosphors have been successfully prepared by an efficient surfactant-free hydrothermal process directly without further sintering treatment. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy-dispersive X-ray (EDS) spectrometry, selected area electron diffraction (SAED), photoluminescence (PL) spectra were used to characterize the samples. The as-obtained samples present flowerlike agglomerates composed of nanoflakes with thickness of 20 nm and high crystallinity in spite of the moderate reaction temperature of 180 °C. The reaction mechanism has been considered as a dissolution/precipitation mechanism; the self-assembly evolution process has been proposed on homocentric layer-by-layer growth style. The different luminescent intensity with different molar ratio of Y-Tb [Y:Tb = 8:2; 7:3; 6:4; 5:5; 4:6], YBO₃:Tb³⁺ phosphors exhibit different light (white, red, green) under ultraviolet excitation, which might find potential applications in the fields such as light display systems and optoelectronic devices.     

Direct synthesis of Fe3O4 nanopowder by thermal decomposition of Fe-urea complex and its properties

An easy synthesis route of magnetite (Fe₃O₄) nanopowder is developed by using thermal decomposition of Fe-urea complex ([Fe(CON₂H₄)₆](NO₃)₃). The formation of Fe₃O₄ is confirmed from X-ray powder diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) measurements. The morphological properties and magnetic properties of the Fe₃O₄ are characterized by transmission electron microscopy (TEM) and magnetic measurements, respectively. By an increase in reaction temperature from 200 to 300 °C, the average crystallite size of the Fe₃O₄ nanopowder increases from 37 to 50 nm. Room temperature magnetization hysteresis curves show that the Fe₃O₄ nanopowder possesses ferrimagnetic characteristics. The saturation magnetization of the Fe₃O₄ nanopowder increases from 70.7 to 89.1 emu/g when the reaction temperature increases from 200 to 300 °C.     

Mechanochemical synthesis of Al2O3-TiB2 nanocomposite powder from Al-TiO2-H3BO3 mixture

Alumina-titanium diboride nanocomposite (Al₂O₃-TiB₂) was produced using mixtures of titanium dioxide, acid boric and pure aluminum as raw materials via mechanochemical process. The phase transformation and structural characterization during mechanochemical process were utilized by X-ray diffractometry (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), and thermogravimetric analyses (TG-DTA) techniques. A thermodynamic appraisal showed that the reaction between TiO₂, B₂O₃ and Al is highly exothermic and should be self-sustaining. XRD analyses exhibited that the Al₂O₃-TiB₂ nanocomposite was formed after 1.5 h milling time. The results indicate that increasing milling time up to 40 h had no significant effect other than refining the crystallite size.     

Preparation and characteristics of Fe3O4@YVO4:Eu bifunctional magnetic-luminescent nanocomposites

A facile direct precipitation method has been developed for the synthesis of bifunctional magnetic-luminescent nanocomposites with Fe₃O₄ nanoparticles as the core and YVO₄:Eu³⁺ as the shell. Transmission electron microscopy (TEM) images revealed that the obtained bifunctional nanocomposites had a core-shell structure and a spherical morphology. The average size was ∼150 nm, and the thickness of the shell was ∼15 nm. The X-ray diffraction (XRD) patterns showed that a cubic spinel structure of Fe₃O₄ core and a tetragonal phase of YVO₄ shell were obtained. Fourier transform infrared (FT-IR) spectra confirmed that the YVO₄:Eu³⁺ had been successfully deposited on the surface of Fe₃O₄ nanoparticles. Photoluminescence (PL) spectra indicated that the nanocomposites displayed a strong red characteristic emission of Eu³⁺. Magnetic measurements showed that the obtained bifunctional nanocomposites exhibited superparamagnetic behavior at room temperature. Therefore, the bifunctional nanocomposites are expected to develop many potential applications in biomedical fields.     

Ultrasonic-assisted in situ synthesis and characterization of superparamagnetic Fe3O4 nanoparticles

Superparamagnetic Fe₃O₄ nanoparticles were synthesized via a modified coprecipitation method, and were characterized with X-ray diffraction (XRD), vibrating sample magnetometer (VSM), Zeta potential and FT-IR, respectively. The influences of different kinds of surfactants (sodium dodecyl benzene sulfonate, polyethyleneglycol, oleic acid and dextran), temperatures and pH values on the grain size and properties were also investigated. In this method, Fe³⁺ was used as the only Fe source and partially reduced to Fe²⁺ by the reducing agent with precise content. The following reaction between Fe³⁺, Fe²⁺ and hydroxide radical brought pure Fe₃O₄ nanoparticles. The tiny fresh nanoparticles were coated in situ with surfactant under the action of sonication. Comparing with uncoated sample, the mean grain size and saturation magnetization of coated Fe₃O₄ nanoparticles decrease from 18.4 nm to 5.9-9.0 nm, and from 63.89 emu g⁻¹ to 52-58 emu g⁻¹ respectively. When oleic was used as the surfactant, the mean grain size of Fe₃O₄ nanoparticles firstly decreases with the increase of reaction temperature, but when the temperature is exceed to 80 °C, the continuous increase of temperature resulted in larger nanoparticles. the grain size decreases gradually with the increasing of pH values, and it remains unchanged when the PH value is up to 11. The saturation magnetization of as-prepared Fe₃O₄ nanoparticles always decreases with the fall of grain size.     

Low temperature synthesis of Fe3O4 micro-spheres and its application in lithium ion battery

Fe₃O₄ micro-spheres with nanoparticles close-packed architectures were synthesized via a simple chemical method using (NH₄)₂Fe(SO₄)₂·6H₂O, hexamethylenetetramine, and NaF as reaction materials. This chemical synthesis took place in a vitreous jar under low temperature (90 °C) and atmospheric pressure. The morphology and structure of the as-synthesized products were characterized by field emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD), and Raman spectrum. Electrochemical properties of the as-synthesized Fe₃O₄ micro-spheres as anode electrode of lithium ion batteries were studied by conventional charge/discharge tests, which exhibit steady charge/discharge platforms at different current densities. The as-prepared Fe₃O₄ electrode shows high initial discharge capacity of 1166 and 1082 mAh g⁻¹ at current density of 0.05 and 0.1 mA cm⁻², respectively.     

Influence of MnO2 on the sintering behavior and magnetic properties of NiFe2O4 ferrite ceramics

The samples with small amounts of MnO₂ (0, 0.5, 1.0, 1.5, 2.0, and 2.5 wt%, respectively) were prepared via ball-milling process and two-step sintering process from commercial powders (i.e. Fe₂O₃, NiO and MnO₂). Microstructural features, phase transformation, sintering behavior and magnetic properties of Mn-doped NiFe₂O₄ composite ceramics have been investigated by means of scanning electron microscopy (SEM), differential thermal analyzer, X-ray diffraction (XRD), thermal dilatometer and vibrating sample magnetometer (VSM) respectively. The XRD analysis and the result of differential thermal analysis indicate that the reduction of MnO₂ into Mn₂O₃ and the following reduction of Mn₂O₃ into MnO existed in sintering process. No new phases are detected in the ceramic matrix, the crystalline structure of the ceramic matrix is still NiFe₂O₄ spinel structure. Morphology and the detecting result of thermal dilatometer show that MnO₂ can promote the sintering process, the temperature for 1 wt% MnO₂-doped samples to reach the maximum shrinkage rate is 59 °C lower than that of un-doped samples. For 1 wt% MnO₂-doped samples, the value of the saturation magnetization (M_s) and coercivity (H_c) is 15.673 emu/g and 48.316 Oe respectively.     

Photocatalytic performance of nano-photocatalyst from TiO2 and Fe2O3 by mechanochemical synthesis

Nano-particles of homogeneous solid solution between TiO₂ and Fe₂O₃ (up to 10 mol%) have been prepared by mechanochemical milling of TiO₂ and yellow Fe₂O₃/red Fe₂O₃/precipitated Fe (OH)₃ using a planetary ball mill. Such novel solid solution cannot be prepared by conventional co-precipitation technique. A preliminary investigation of photocatalytic activity of mixed oxide (TiO₂/Fe₂O₃) on photo-oxidation of different organic dyes like Rhodamine B (RB), Methyl orange (MO), Thymol blue (TB) and Bromocresol green (BG) under visible light (300-W Xe lamp; λ > 420 nm) showed that TiO₂ having 5 mol% of Fe₂O₃ (YFT1) is 3-5 times higher photoactive than that of P25 TiO₂. The XRD result did not show the peaks assigned to the Fe components (for example Fe₂O₃, Fe₃O₄, FeO₃, and Fe metal) on the external surface of the anatase structure in the Fe₂O₃/TiO₂ attained through mechanochemical treatment. This meant that Fe components were well incorporated into the TiO₂ anatase structure. The average crystallite size and particle size of YFT1 were found to be 12 nm and 30 ± 5 nm respectively measured from XRD and TEM conforming to nanodimensions. Together with the Fe component, they absorbed wavelength of above 387 nm. The band slightly shifted to the right without tail broadness, which was the UV absorption of Fe oxide in the Fe₂O₃/TiO₂ particle attained through mechanochemical method. This meant that Fe components were well inserted into the framework of the TiO₂ anatase structure. EPR and magnetic susceptibility show that Fe³⁺ is in low spin state corresponding to μ_B = 1.8 BM. The temperature variation of μ_B shows that Fe³⁺ is well separated from each other and does not have any antiferromagnetic or ferromagnetic interaction. The evidence of Fe³⁺ in TiO₂/Fe₂O₃ alloy is also proved by a new method that is redox titration which is again support by the XPS spectrum.     

Synthesis of lanthanum carbonate nanoparticles via sonochemical method for preparation of lanthanum hydroxide and lanthanum oxide nanoparticles

Lanthanum carbonate nanoparticles were synthesized from the reaction of lanthanum acetate and Na₂CO₃ under sonication via sonochemical method. Lanthanum hydroxide nanoparticles were prepared by facial hydrothermal processing from the resulted product at 110 °C for 24 h. The role of surfactant, calcination temperature and sonication time were investigated on the morphology and particle size of the products. Products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectrum (XPS), and Fourier transform infrared (FT-IR) spectra. La₂O₃ nanoparticles were obtained by calcinations of the nanoparticles of lanthanum carbonate at 600 °C.     

Electromagnetic composite films based on polypyrrole hydro-sponge and Fe3O4 ferrofluid

The preparation of free-standing electromagnetic composite films based on conductive polypyrrole (PPy) hydro-sponge and the Fe₃O₄ ferrofluid have been successfully accomplished via self-assembly in the presence of β-cyclodextrin sulfate and under static condition. Transmission electron microscope (TEM), scanning electron microscope (SEM) and X-ray diffraction (XRD) are used to study the morphology of the PPy-Fe₃O₄ composite. Structural characterizations by Fourier transform infrared (FTIR) and thermogravimetric analysis (TGA) have proved the interactions between Fe₃O₄ and PPy chains. As-prepared films possess high electrical conductivity, remarkable magnetic response as well as appropriate flexility. Both the conductivity and magnetization of the composite, the latter in particular, depend strongly on the Fe₃O₄ content and thus can be optimized by adjusting the relative content of Fe₃O₄ in the composite. The combination of both magnetic and conducting activities of the resulting composite makes it be a potential candidate as functional material in electromagnetic devices, such as magnetic-controlled switches.     

Morphology and phase evolvement of Yb/Er co-doped NaYF4 microtubes prepared with YF3 submicrospindles as precursor

Hexagonal phase NaYF₄ microtubes co-doped with Yb³⁺ and Er³⁺ were synthesized through a hydrothermal process with YF₃ submicrospindles as precursor. The X-ray powder diffraction (XRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM) and high resolution transmission electron microscopy (HRTEM) were utilized to characterize the structure and morphology of the as-prepared products. XRD results show that pure cubic NaYF₄ crystals can be obtained when reaction time is 2 h. While the product is mixture of cubic and hexagonal phase NaYF₄ when reaction time is from 7 to 20 h. Continuing to increase the reaction time to 24 h, the pure hexagonal NaYF₄ crystals were formed. The FE-SEM and TEM results show that the morphology of pure cubic NaYF₄ is spherical clusters composed of spherical nanoparticles with average diameter of about 100 nm and the pure hexagonal NaYF₄ crystals have tubular structure with out diameter of about 0.3-0.5 μm, inner diameter of about 0.5-1 μm and length ranging from 3 to 12 μm. The luminescence properties of Yb³⁺/Er³⁺ co-doped cubic and hexagonal phase NaYF₄ microcrystals were also studied. Under 980-nm excitation, the upconversion luminescence (UCL) intensity of hexagonal phase NaYF₄ microtubes is much stronger than that of cubic phase clusters. Moreover, both red and green upconversion are ascribed to the two-photon process. Therefore, hexagonal phase NaYF₄ microtubes with high UCL efficiency may have a potential application in photonic device.     

Synthesis and characteristics of poly(3-pyrrol-1-ylpropanoic acid) (PPyAA)-Fe3O4 nanocomposite

Poly(3-pyrrol-1-ylpropanoic acid) (PPyAA)-Fe₃O₄ nanocomposite was successfully synthesized by an in situ polymerization of 1-(2-carboxyethyl) pyrrole in the presence of synthesized Fe₃O₄ nanoparticles. Evaluation of structural, morphological, electrical and magnetic properties of the nanocomposite was performed by XRD, FT-IR, TEM, TGA, magnetization and conductivity measurements, respectively. XRD analysis reveals the inorganic phase as Fe₃O₄ and TGA shows about 90 wt% loading of Fe₃O₄ in the nanocomposite. FT-IR analysis indicates a successful conjugation of Fe₃O₄ particles with polypyrrole acetic acid. Magnetization measurements show that polypyrrole acetic acid coating decreases the saturation magnetization of Fe₃O₄ significantly. This reduction has been explained by the pinning of the surface spins by the possible adsorption of non-magnetic ions during the polymerization process. The conductivity and dielectric permittivity measurements strongly depend on the thermally activated polarization mechanism and thermal transition of PPyAA in the nanocomposite structure. Large value of dielectric permittivity (?′) of the nanocomposite at lower frequency is attributed to the predominance of species like Fe²⁺ ions and grain boundary defects (interfacial polarization).     

Synthesis of lanthanum hydroxide and lanthanum oxide nanoparticles by sonochemical method

In this work lanthanum hydroxide nanoparticles were synthesized by sonochemical method. La₂O₃ nanoparticles were obtained after calcination of the La(OH)₃ nanoparticles precursor in air at 600 °C for 2 h. The effect of some parameters such as concentration of precursors, pulse time of sonication, time of sonication, and addition of PEG as surfactant on the morphology and the particle size were studied. The as-prepared products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectrum (XPS) and Fourier transform infrared (FT-IR) spectra.     

Combustion synthesis of CaSc2O4:Ce nano-phosphors in a closed system

The CaSc₂O₄:Ce³⁺ nano-phosphors were successfully prepared by a single-step combustion method at an ignition temperature as low as 200 °C in a closed autoclave using glycine as a fuel and PEG4000 as a dispersant. The samples were characterized by X-ray diffraction (XRD), photoluminescence (PL) spectroscopy, scanning electron microscopy (SEM) and transmission electron microscope (TEM). The results revealed that CaSc₂O₄:Ce³⁺ nano-phosphors can be conveniently prepared at an ignition temperature as low as 200 °C, which was much lower than that in the ordinary combustion methods. The optimized ignition temperature was 220 °C. The CaSc₂O₄:Ce³⁺ nano-phosphors give a uniform particle size in the range of 15-20 nm. The low ignition temperature and the addition of PEG4000 dispersant play important roles in the formation of small sized nanoparticles. The as-prepared nano-phosphors were incompact aggregates, but highly dispersed nano-phosphors can be obtained after further ultrasonic treatment. The CaSc₂O₄:Ce³⁺ nano-phosphors give satisfactory luminescence characteristic benefiting from the closed circumstance, in which cerium atoms can be isolated from the oxidizing atmosphere and non-fluorescent Ce⁴⁺ ions can be ruled out. The present highly dispersed CaSc₂O₄:Ce³⁺ nano-phosphors with efficient fluorescence are promising in the field of biological labeling, and the present low temperature combustion method is facile and convenient and can be applied as a universal process for preparing non-aggregate oxide nano-phosphors, especially those being sensitive to air at high temperature.     

Fabrication of V3O7·H2O@C core-shell nanostructured composites and the effect of V3O7·H2O and V3O7·H2O@C on decomposition of ammonium perchlorate

V₃O₇·H₂O@C core-shell materials have been synthesized using V₃O₇·H₂O nanobelts as the cores and glucose as the source of carbon via an environmental hydrothermal method. The as-obtained V₃O₇·H₂O@C core-shell materials were characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM), elemental analysis (EA), Fourier transform infrared spectroscopy (FT-IR) and Raman spectrum. The influences of the reaction temperature, concentration of glucose and reaction time on the morphologies of the samples were respectively discussed in detail. The possible formation mechanism of V₃O₇·H₂O@C was proposed according to our experimental results. Furthermore, the effect of V₃O₇·H₂O and V₃O₇·H₂O@C on the thermal decomposition of ammonium perchlorate (AP) were investigated by thermal gravimetric analyzer (TG) and differential thermal analysis (DTA). The thermal decomposition temperatures of AP in the presence of V₃O₇·H₂O and V₃O₇·H₂O@C were reduced by 70 and 89 °C, respectively, which indicates that V₃O₇·H₂O@C core-shell composites have higher activity than V₃O₇·H₂O.     

Preparation of CuIn1−xGaxS2 (x = 0.5) flowers consisting of nanoflakes via a solvothermal method

CuIn_1−xGa_xS₂ (x = 0.5) flowers consisting of nanoflakes were successfully prepared by a biomolecule-assisted solvothermal route at 220 °C for 10 h, employing copper chloride, gallium chloride, indium chloride and l-cysteine as precursors. The biomolecule l-cysteine acting as sulfur source was found to play a very important role in the formation of the final product. The diameter of the CuIn_0.5Ga_0.5S₂ flowers was 1-2 μm, and the thickness of the flakes was about 15 nm. The obtained products were characterized by X-ray diffraction (XRD), energy dispersion spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), field-emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), selected area electron diffraction spectroscopy (SAED), and UV-vis absorption spectroscopy. The influences of the reaction temperature, reaction time, sulfur source and the molar ratio of Cu-to-l-cysteine (reactants) on the formation of the target compound were investigated. The formation mechanism of the CuIn_0.5Ga_0.5S₂ flowers consisting of flakes was discussed.     

Characterisation of the coke formed during metal dusting of iron in CO-H2-H2O gas mixtures

Carbon deposits formed on the surface of iron samples during carburisation at 700 °C in a gas mixture of 75%CO-24.81%H₂-0.19%H₂O were characterised by using scanning electron microscopy (SEM), X-ray diffraction (XRD), Mössbauer spectroscopy and transmission electron microscopy (TEM). Cross-section observation of the iron sample by light optical microscopy revealed the formation of cementite after only 10 min reaction, together with a thin layer of graphite. After 4 h reaction, a thick coke layer was formed on top of the cementite surface. SEM surface observation indicated the formation of filamentous carbon in the coke layer. Further analysis of the coke by XRD and Mössbauer showed the presence of mainly Fe₃C and small amount of Fe₂C but no metallic iron in the carbon deposit. TEM analysis of the coke detected very convoluted filaments with iron-containing particles at the tip or along their length. These particles were identified to be cementite by selected area diffraction. Carbon deposits produced at the same temperature but with other gas compositions were also analysed by using XRD. It was found that with a low content of CO, e.g. 5%, both α-Fe and Fe₃C were detected in the coke. Increasing CO content to more than 30%, iron carbide was the only iron-containing phase.