Synthesis and acetone gas sensing properties of Ag activated hollow sphere structured ZnFe2O4

Sheet stacked ZnFe₂O₄ hollow spheres have been synthesized through a simple hydrothermal method using Zn(CH₃COO)₂ and Fe(NO₃)₃ as Zn and Fe sources, respectively. Then a series of Ag activated ZnFe₂O₄ composites are prepared. XRD patterns demonstrate that the as-synthesized powders are pure ZnFe₂O₄. FE-SEM images exhibit that the as-synthesized Ag-ZnFe₂O₄ particles are spherical with the diameter of 800–1000?nm. TEM images demonstrate that the as-synthesized Ag-ZnFe₂O₄ are hollow sphere structure. The gas sensing tests show that 0.25?wt% Ag-ZnFe₂O₄ has the highest responses to 100?ppm acetone vapor at 175?°C, and response time and recovery time are 17 and 148?s respectively. In addition, 0.25?wt% Ag-ZnFe₂O₄ has a good selectivity to acetone. Ag activated ZnFe₂O₄ composites exhibit excellent acetone gas sensing properties and gives potential for the detection of acetone vapor in the application of practical industrial processes and health control.     

Mechanochemical synthesis of zinc ferrite from zinc oxide and α-Fe2O3

Mechanochemical synthesis of zinc ferrite (ZnFe₂O₄) from a powder mixture of zinc oxide (ZnO) and hematite (α-Fe₂O₃) by room temperature grinding using a planetary ball mill was investigated. The grinding enables us to obtain the amorphous mixture of the starting materials. Most of ZnO reacts with α-Fe₂O₃ to convert into insoluble amorphous zinc and iron compounds within 2h-grinding. Prolonged grinding enhances the crystallization of ZnFe₂O₄ from the amorphous compounds. ZnFe₂O₄ crystallized by the grinding for 3 h or more consists of nanocrystalline particles with high specific surface area.     

Microwave synthesis of magnetically separable ZnFe2O4-reduced graphene oxide for wastewater treatment

A magnetically separable ZnFe₂O₄-reduced graphene oxide (rGO) nano-composite was synthesised via a microwave method. Field emission scanning electron microscopy images of the nano-composite showed a uniform dispersion of nanoparticles on the rGO sheets. The performance of the nano-composite in wastewater treatment was assessed by observing the decomposition of methylene blue. The nano-composite showed excellent bifunctionality, i.e. adsorption and photocatalytic degradation of methylene blue, for up to five cycles of water treatment when illuminated with light from a halogen bulb. In contrast, water treatment with the nano-composite without illumination and the illuminated rGO, with no decoration of nanoparticles, diminished significantly after the first treatment. The reclamation of the ZnFe₂O₄-rGO nano-composite from treated water could be easily achieved by applying an external magnetic field.     

Fast synthesis of MgAl2O4‒W and MgAl2O4‒W‒W2B composite powders by self-propagating high-temperature synthesis reactions

MgAl₂O₄?W and MgAl₂O₄?W?W₂B composite powders were obtained rapidly in a single step by self-propagating high-temperature synthesis of WO₃?Mg?xAl₂O₃ and WO₃?B₂O₃?Mg?yAl₂O₃ systems. The addition of various Al₂O₃ contents (x and y-values) to the starting materials was considered as the main synthesis parameter. Thermodynamic calculations revealed that the adiabatic temperature of both systems was decreased with increasing Al₂O₃ content. The XRD results indicated that after acid leaching of the WO₃?Mg?xAl₂O₃ combustion products, W and MgAl₂O₄ were formed as the main phases and WO₂, MgWO₄ and Al₂O₃ as the minor constituents in the final composite. On the other hand, MgAl₂O₄?W composites were synthesized in the WO₃?B₂O₃?Mg?yAl₂O₃ system at y<1.4 mol. By increasing the y-value to 2.1 mol, W₂B was formed as a new product leading to production of MgAl₂O₄?W?W₂B composite. The formation of spinel was confirmed by the Fourier transformed infrared spectroscopy analysis. Microstructure observations represented the uniform distribution of MgAl₂O₄ blocks within the fine spherical W particles. The melting of Al₂O₃ was found as a vital step for rapid synthesis of MgAl₂O₃ by the SHS route. Finally, the possible formation mechanism of MgAl₂O₄ during the combustion synthesis was proposed.     

Synthesis of MFe2O4 (M=Mg2+, Zn2+, Mn2+) spinel ferrites and their structural,elastic and electron magnetic resonance properties

Structural, elastic and electron magnetic resonance investigations of spinel ferrites with the formula MFe₂O₄ (M = Mg²⁺, Zn²⁺, Mn²⁺) synthesized by the sol-gel auto-combustion method are reported here. XRD patterns revealed the co-existence of secondary phases along with the ferrite phase. The lattice parameter (8.301?Å, 8.366?Å and 8.434?Å) was found to be varying according to the ionic radii of cations. As determined by scanning electron microscopy (SEM), ZnFe₂O₄ has a comparatively narrow distribution of grain sizes (1.3–3.8?µm) compared to those in MnFe₂O₄ (0.8–4.3?µm) and MgFe₂O₄ (0.3–4.8?µm). The estimated values of average crystallite sizes (17.5?nm, 21.3?nm and 23.3?nm) determined from the X-ray diffraction peaks are considerably less than the average grain sizes (1.3?µm, 1.6?µm and 2.7?µm) estimated from the SEM histograms. The vibrational frequencies in FTIR spectra are in the conformity with the cubic spinel structure and their variation supports the variation of lattice parameter. Equal values of Poission's ratio (0.35) were obtained for the three systems which represent the isotropic behaviour of spinel ferrite systems. The exceptional low value of Lande's g-parameter for ZnFe₂O₄ indicates the dominance of Fe³⁺–O–Fe³⁺ superexchange interaction. Though cation redistribution is possible in the present ferrite systems, the secondary phases existed in these ferrite systems are predominantly influencing the structural, elastic and electron magnetic resonance properties.     

Structure and magnetic properties of multi-morphological CoFe2O4/CoFe nanocomposites by one-step hydrothermal synthesis

Multi-morphological CoFe₂O₄/CoFe nanocomposites have been synthesized using a facile hydrothermal process. The effects of hydrazine hydrate amount during hydrothermal reaction on the structure and magnetic property of the specimens were studied. With increasing hydrazine hydrate amount, the CoFe₂O₄ transformed to CoFe and the morphology of the specimen changed from granular particles to faceted particles. The saturation magnetization monotonically increased and the coercivity monotonically decreased with increasing hydrazine hydrate amount. The magnetic interactions, determining the magnetic properties of the composites, result from the dominant dipole coupling and relative weak exchange coupling between CoFe₂O₄ and CoFe nanoparticles. The CoFe₂O₄/CoFe nanocomposite prepared with 2?mL hydrazine hydrate exhibited the optimal magnetic properties, with the saturation magnetization of 81?emu/g and coercivity of 636?Oe.     

Synthesis and characterization of poly(styrene-co-fluorescein O-methacrylate)/poly(N-isopropylacrylamide)-Fe3O4 core/shell composite particles

We demonstrate the synthesis and characteristics of multifunctional poly(styrene-co-fluorescein O-methacrylate)/poly(N-isopropylacrylamide)-Fe₃O₄ [P(St/FMA)/PNIPAAm-Fe₃O₄] core/shell composite particles, in which the core consists of fluorescent materials and the shell consists of magnetic and thermo-responsive components. First, core/shell particles consisting of a fluorescent P(St/FMA) core and thermo-responsive PNIPAAm-rich shell were prepared by two-stage shot-growth emulsion polymerization. Next, Fe₃O₄ nanoparticles were immobilized via electrostatic interactions and then covalently linked to the shell via surface coordinated Aphen by a coupling reaction in order to obtain magnetic properties. The morphology of P(St/FMA)/PNIPAAm-Fe₃O₄ composite particles, confirmed by transmission electron microscopy (TEM), reveals that Fe₃O₄ nanoparticles are located in the PNIPAAm shell. The thermo-sensitivity of composite particles to hydrodynamic diameter was confirmed by using dynamic light scattering (DLS). Photoluminescence (PL) spectra indicate that the fluorescence emission intensity of core/shell particles is highly sensitive to the pH of an aqueous medium. The core/shell composite particles exhibited a combination of fluorescent, magnetic, pH and thermo-responsive behavior.     

One-step room-temperature solid-phase synthesis of ZnFe2O4 nanomaterials and its excellent gas-sensing property

ZnFe₂O₄ nanomaterials have been synthesized by simple one-step solid-phase chemical reaction between Zn(CH₃COO)₂·2H₂O, FeCl₃·9H₂O and NaOH within a very short time at room temperature. The solid-phase products were characterized by X-ray diffraction, energy-dispersive X-ray spectroscopy, thermogravimetic analysis, transmission electron microscopy and scanning electron microscopy. Results indicated that the particle size of product can be obviously let up and the agglomeration phenomenon can be improved by the surfactant. Moreover, the ZnFe₂O₄ nanomaterials were applied in gas sensor and exhibited much better sensing performance than bulk ZnFe₂O₄. The as-prepared ZnFe₂O₄ nanomaterials have high sensitivity, good selectivity and fast response/recovery characteristic for ethanol and hydrogen sulfide. The improved ZnFe₂O₄ nanomaterials have high response value of 21.5 and 14.8 for ethanol and hydrogen sulfide in the optimized operating temperature of 332 °C and 240 °C, respectively. The response and recovery time was found to be within 4 s and 14 s for ethanol, while 7 s and 25 s for hydrogen sulfide.     

Enhanced gyromagnetic properties of NiCuZn ferrite ceramics for LTCC applications by adjusting MnO2-Bi2O3 substitution

The demand for high performance microwave devices is increasingly promoting the development of miniaturization, integration and multifunctionalization. Here, a uniform and dense NiCuZn ferrite ceramic with high saturation magnetization and low ferromagnetic resonance linewidth was obtained at 950?°C by adjusting the MnO₂-Bi₂O₃ composite additives. The MnO₂-Bi₂O₃ composite additives were composed of 0.5?wt% MnO₂ and x wt% Bi₂O₃ (x?=?0.0, 0.5, 1.0, 1.5, 2.0, and 3.0). The phase structure, microstructures and magnetic properties were systematically studied by means of modern measurement techniques. SEM images reveal that appropriate MnO₂-Bi₂O₃ additions can promote grain growth and reduce sintering temperatures, which is very advantageous for LTCC technology. In addition, the content of MnO₂-Bi₂O₃ additives can significantly reduce ferromagnetic resonance linewidth (FMR) by promoting grain growth and densification at low temperatures. Finally, a uniform and compact NiCuZn ferrite ceramic with an improved 4πM_s (~?3812.5 Gauss), a narrow ΔH (~?144.6?Oe), and a reduced H_c (~?85.2?A/m) were obtained (at 950?°C) by adding the optimal volume of Bi₂O₃ additive. It is expected that the improved gyromagnetic performances will allow the NiCuZn ferrite ceramics to be promising candidates for X-band microwave devices.     

Synthesis and magnetic properties of monodisperse CoFe2O4 nanoparticles coated by SiO2

The monodisperse CoFe₂O₄ nanoparticles were synthesized by a modified chemical coprecipitation method. Coating SiO₂ on the surface of the CoFe₂O₄ nanoparticles was carried out to keep single domain particles non-interacting with cubic magnetocrystalline anisotropy. The Curie temperatures (T_c) of the monodisperse CoFe₂O₄ nanoparticles can be accurately measured because the SiO₂ shells prevented the aggregation and growth of nanoparticles at high temperature. The magnetic properties of the CoFe₂O₄@SiO₂ nanoparticles with core-shell structure in a wide temperature range (300～950?K) were investigated. It is remarkable that the coercive field (H_c) of CoFe₂O₄ nanoparticles increased from about 760?Oe to 1806?Oe after being coated with SiO₂, which increased by 137.6% compared to the uncoated samples at 300?K. The saturation magnetization (M_s) of the CoFe₂O₄@SiO₂ nanoparticles is 34.59?emu/g, which is about 52% of the naked CoFe₂O₄ nanoparticles value (66.51?emu/g) at 300?K. The hysteresis loops of the CoFe₂O₄@SiO₂ nanoparticles showed an orderly magnetic behavior at high temperature, such as the M_s, remanence magnetization (M_r) and H_c decreased as temperature increasing, being equal to zero near T_c. This is a good indication that the CoFe₂O₄@SiO₂ nanoparticles are suitable for a wide variety of technological applications at high temperature.     

Magnetic and Optical Properties of Mn1−xZnxFe2O4 Nanoparticles

Mn_1?xZn_xFe₂O₄ (x = 0.0?1.0) NPs (MZF NPs) were synthesized by a citric acid assisted sol–gel process. MZF NPs show superparamagnetic characteristics at room temperature. Saturation magnetization (M_s) of MnFe₂O₄ NPs is 70.52 emu/g is very close to the bulk saturation magnetization value of 80 emu/g. The observed M_s = 35.90 emu/g value for ZnFe₂O₄ particles is much greater than the bulk M_s value of 5 emu/g. This case is attributed to cation distribution change from normal spinel to mixed structure. The small M_r/M_s ratios (the maximum 0.147) specify uniaxial anisotropy in the Mn_1-xZn_xFe₂O₄ NPs. The average crystallite diameter (D _mag) was evaluated from magnetic analyses. The obtained D _mag values are between 27.67 and 33.60 nm and this range is in great accordance with the results calculated from XRD measurements. Among the NPs, the samples with more zinc content show higher diffuse reflectance. The optical direct band gap of MZF NPs is found to decrease from 2.1 to 1.90 eV as the zinc content rises.     

Synthesis and magnetic properties of CoAlFe2O4 nanoparticles

Nanosized particles of CoAl_xFe_2-xO₄, where 0?≤?x?≤?2, were synthesized by the sol–gel combustion method and the magnetic properties of these compounds were investigated. According to X-ray diffractograms, the samples are single phase and the crystallite size is between 7 and 25?nm. The room temperature saturation magnetization of the samples was estimated from the cation distribution and ferromagnetic resonance spectra were used to determine the magnetocrystalline anisotropy. The results show that the saturation magnetization and the magnetocrystalline anisotropy vary over a wide range, from maxima of M_s =?0.42?MA/m and K?=?0.39?kJ/m³ for x?=?1.0 to minima of almost zero for x?≈?1.4, a result that could be useful for practical applications of these materials.     

Effect of CsxH3?xPW12O40 addition on the catalytic performance of ZnFe2O4 in the oxidative dehydrogenation of n-butene to 1,3-butadiene

Oxidative dehydrogenation of n-butene to 1,3-butadiene over ZnFe₂O₄ catalyst mixed with Cs _x H_3−x PW₁₂O₄₀ heteropolyacid (HPA) was performed in a continuous flow fixed-bed reactor. The effect of Cs _x H_3−x PW₁₂O₄₀ addition on the catalytic performance of ZnFe₂O₄ was investigated. Cs _x H_3−x PW₁₂O₄₀ itself showed very low catalytic performance in the oxidative dehydrogenation of n-butene. However, addition of small amount of Cs _x H_3−x PW₁₂O₄₀ into ZnFe₂O₄ enhanced the catalytic performance of ZnFe₂O₄ catalyst. The catalytic performance of ZnFe₂O₄-Cs _x H_3−x PW₁₂O₄₀ mixed catalysts was closely related to the surface acidity of Cs _x H_3−x PW₁₂O₄₀. Among the catalysts tested, ZnFe₂O₄-Cs_2.5H_0.5 PW₁₂O₄₀ mixed catalyst showed the best catalytic performance. Strong acid strength and large surface acidity of Cs_2.5H_0.5PW₁₂O₄₀ was responsible for high catalytic performance of ZnFe₂O₄-Cs_2.5H_0.5PW₁₂O₄₀ mixed catalyst. Thus, Cs_2.5H_0.5PW₁₂O₄₀ could be utilized as an efficient promoter and diluent in formulating ZnFe₂O₄ catalyst for the oxidative dehydrogenation of n-butene.     

Carbothermal synthesis of approximately spherical Si3N4 particles with homogeneous size distribution

Si₃N₄ particles with approximately spherical appearance, good dispersity, and homogeneous particle size distribution were successfully fabricated by a modified carbothermal method with the use of high-pressure N₂ and composite additives CaF₂ and Y₂O₃. The effects of parameters such as N₂ gas pressure, additive, and temperature on the carbothermal reduction-nitridation (CRN) process were examined in detail. Based on extensive investigations, the mechanism of formation of Si₃N₄ particles was revealed. It was found that the process of nucleation and growth of Si₃N₄via the vapour-liquid-solid (V-L-S) mechanism under sufficient liquid encapsulation was essential for synthesising uniform particles with approximately spherical morphology and good dispersity. Because of the favourable morphology, the as-prepared Si₃N₄ particles exhibited great potential as thermally conductive fillers for next generation thermal interface materials.     

Synthesis and strengthened microwave absorption properties of three-dimensional porous Fe3O4/graphene composite foam

The three-dimensional porous Fe₃O₄/graphene composite foam as a new kind of absorbing composite with electrical loss and magnetic loss was successfully synthesized by a facile method. Fe₃O₄ was evenly attached on structure of graphene sheets which overlapped with each other to form three-dimensional porous graphene foam. The results revealed that when the mass ratio of graphene oxide (GO) and Fe₃O₄ was 1:1, the Fe₃O₄/graphene composite foam possessed the best absorption properties: the minimum reflection loss was up to ??45.08?dB when the thickness was 2.5?mm and the bandwidth below ??10?dB was 6.7?GHz when the content of the composite foam absorbents was just 8%. The micron-sized three-dimensional porous structure provided more propagation paths, enhancing the energy conversion of incident electromagnetic waves. The addition of Fe₃O₄ contributed to improving the impedance matching performance and magnetic loss. The three-dimensional porous Fe₃O₄/graphene composite foam was a kind of high-efficiency wave absorber, providing a new idea for the development of microwave absorbing materials.     

Photocatalytic and antibacterial activity of PVA mediated Zinc–Zirconium ferrite composites

In this work, Novel zinc-zirconium ferrite (ZnFe₂O₄/ZrFe₂O₅) composite and Zinc ferrite/zirconia (ZnFe₂O₄/ZrO₂) composite were synthesized via coprecipitation technique using Polyvinyl alcohol (PVA) as surfactant. The crystalline structures of the samples were revealed by X-ray diffraction technique. The crystallite sizes were in the range of 50–70 nm. The morphology and elemental composition were studied using scanning electron microscopy, where the zinc ferrite had a truncated octahedral structure with zirconium ferrite decorated on it. The optical properties analyzed through diffuse reflectance spectroscopy and photoluminescence spectroscopy revealed that the samples had good UV and Visible light responses and had oxygen vacancies. The oxygen vacancies enhanced the photocatalytic degradation of methylene blue studied under sunlight and halogen lamp. The vibrating sample magnetometer (VSM) analysis corroborates the ferrimagnetic nature of the composites. The antibacterial activity against Escherichia coli and Staphylococcus aureus was also examined and compared with the commercial antibiotic, amikacin, and other ferrite-composites reported.     

Development of hard/soft ferrite nanocomposite for enhanced microwave absorption

Nickel and zinc substituted strontium hexaferrite, SrFe₁₁Zn_0.5Ni_0.5O₁₉ (SrFe₁₂O₁₉/NiFe₂O₄/ZnFe₂O₄) nanoparticles having super paramagnetic nature are synthesized by co-precipitation of chloride salts using 7.5 M sodium hydroxide solution. The resulting precursors are heat treated (HT) at 900 and 1200 °C for 4 h in nitrogen atmosphere. During heat treatment, transformation proceeds as a constant rate of nucleation and three dimensional growth with an activation energy of 176.79 kJ/mol. The hysteresis loops show an increase in saturation magnetization from 1.042 to 59.789 emu/g with increasing HT temperatures. The ‘as-synthesized’ particles with spherical and needle shapes have size in the range of 20–25 nm. Further, these spherical and needle shaped nanoparticles tend to change their morphology to hexagonal plate and pyramidal shapes with increase in HT temperatures. The effect of such a systematic morphological transformation of nanoparticles on dielectric (complex permittivity and permeability) and microwave absorption properties are estimated in X band (8.2–12.2 GHz). The maximum reflection loss of the composite reaches −29.62 dB (99% power attenuation) at 10.21 GHz which suits its application in RADAR absorbing materials.     

Synthesis and physical characteristics of ZnAl2O4 nanocrystalline and ZnAl2O4/Eu core-shell structure via hydrothermal route

Nanocrystalline zinc aluminate (ZnAl₂O₄) particles with a spinel structure were prepared by hydrolyzing a mixture of aluminum chloride hexahydrate and zinc chloride in deionized water. It was found that pH value and reaction temperature play critical roles in the formation of nano-sized ZnAl₂O₄. Depending on pH values in the precursor solution, ZnAl layered double hydroxide (ZnAl-LDH), ZnO, boehmite or gibbsite could be formed. At pH 7 and T>120 °C, the nanocrystalline ZnAl₂O₄ particles with average particle size of ∼5 nm are easily synthesized through ZnAl layered double hydroxide (ZnAl-LDH). After surface treatment with R-OH by using the cationic surfactant CTAB, the ZnAl₂O₄/Eu core-shell structure can be developed. The ZnAl₂O₄/Eu core-shell structure can show both emissions from ⁵D₀ to ⁷F₂ sensitivity energy level and ⁵D₂ to ⁷F₀ depth energy level.     

High-rate characteristics of novel anode Li4Ti5O12/polyacene materials for Li-ion secondary batteries

In recent years, spinel lithium titanate (Li₄Ti₅O₁₂) as a superior anode material for energy storage battery has attracted a great deal of attention because of the excellent Li-ion insertion and extraction reversibility. However, the high-rate characteristics of this material should be improved if it is used as an active material in large batteries. One effective way to achieve this is to prepare electrode materials coated with carbon. A Li₄Ti₅O₁₂/polyacene (PAS) composite were first prepared via an in situ carbonization of phenol-formaldehyde (PF) resin route to form carbon-based composite. The SEM showed that the Li₄Ti₅O₁₂ particles in the composite were more rounded and smaller than the pristine one. The PAS was uniformly dispersed between the Li₄Ti₅O₁₂ particles, which improved the electrical contact between the corresponding Li₄Ti₅O₁₂ particles, and hence the electronic conductivity of composite material. The electronic conductivity of Li₄Ti₅O₁₂/PAS composite is 10⁻¹ S cm⁻¹, which is much higher than 10⁻⁹ S cm⁻¹ of the pristine Li₄Ti₅O₁₂. High specific capacity, especially better high-rate performance was achieved with this Li₄Ti₅O₁₂/PAS electrode material. The initial specific capacity of the sample is 144 mAh/g at 3 C, and it is still 126.2 mAh/g after 200 cycles. By increasing the current density, the sample still maintains excellent cycle performance.     

Photocatalytic Decolorization of Congo Red Wastewater by Magnetic ZnFe2O4/Graphene Nanosheets Composite under Simulated Solar Light Irradiation

ABSTRACT

ZnFe₂O₄ supported on graphene nanosheets (ZnFe₂O₄@GNs) was prepared by a one-step hydrothermal method. Characterization results of XRD and SEM demonstrated that ZnFe₂O₄ has been anchored on the surface of graphene nanosheets. After four successive cycles, removal efficiency of congo red is 88.66% by ZnFe₂O₄@GNs while 39.80% by ZnFe₂O₄, suggesting high photocatalytic stability of ZnFe₂O₄@GNs under simulated solar light. Quenching experiments confirmed that h⁺ generated is the primary oxidizing agent, while both ?OH and O₂^?? reactive species are also involved for the photodegradation of organic dye pollutants. ZnFe₂O₄@GNs can be easily separated from the reacted aqueous solution using magnetic field. Results indicate the potential applications of ZnFe₂O₄@GNs in effective removal of organic dye wastewater.