Effect of the thermal treatment conditions on the formation of zinc ferrite nanocomposite, ZnFe2O4, by sol–gel method

Zinc ferrite nanocomposite was synthesized via thermal decomposition of zinc acetate and iron nitrate at three different temperatures (350, 450, and 550 °C). The influence of the thermal decomposition of precursors on the formation zinc ferrites was studied by differential thermal gravimetry and thermogravimetry (TG). The TG curve shows two steps for the thermal decomposition with mass loss of 17.3 % at 78 °C and 63.3 % at 315 °C. The prepared zinc ferrites nanocomposite was characterized by X-ray diffraction and scanning electron microscopy. The X-ray diffractograms of ZnFe₂O₄ shows that a crystalline phase, spinel system is formed. SEM micrograph of the zinc ferrite nanocomposite indicates the formation of uniformly spherical 48-nm nanograins. The properties of the zinc ferrite phase were strongly dependent on their calcinations temperature and molar ratio of precursors.     

Surfactant Assisted Hydrothermal Synthesis of Superparamagnetic ZnFe<Subscript>2</Subscript>O<Subscript>4</Subscript> Nanoparticles as an Efficient Visible-Light Photocatalyst for the Degradation of Organic Pollutant

Super paramagnetic ZnFe₂O₄ nanoparticles were prepared by a surfactant assisted (ethylamine) hydrothermal method along with heat treatment. The nanoparticles were characterized by X-ray diffraction, Fourier transform infrared spectroscopy, high resolution scanning electron microscopy, Transmission electron microscopy, vibrating sample magnetometer and diffuse reflectance spectra technique. From the analyses, influence of calcination temperature on the structural, vibrational, morphological, magnetic and optical properties of ZnFe₂O₄ nanoparticles were investigated. The ZnFe₂O₄ nanoparticles with an average particle size of 17 nm showed high photocatalytic activity in the degradation of methylene blue (90 %). This work demonstrates that ZnFe₂O4 can be used as a potential monocomponent in visible-light photocatalysis for the degradation of organic pollutants. Furthermore, the products were super paramagnetic and could be conveniently separated within 15 min and recycled by using simple magnet, which is very beneficial for the degradation of organic pollutants.     

Graphene anchored with ZnFe2O4 nanoparticles as a high-capacity anode material for lithium-ion batteries

Heterostructured ZnFe₂O₄–graphene nanocomposites are synthesized by a facile hydrothermal method. The as-prepared ZnFe₂O₄–graphene nanocomposites are characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), Brunauer–Emmett–Teller (BET) analysis and galvanostatic charge and discharge measurements. Compared with the pure ZnFe₂O₄ nanoparticles, the ZnFe₂O₄–graphene nanocomposites exhibit much larger reversible capacity up to 980 mAh g⁻¹, greatly improved cycling stability, and excellent rate capability. The superior electrochemical performance of the ZnFe₂O₄–graphene nanocomposites could be attributed to the synergetic effect between the conducting graphene nanosheets and the ZnFe₂O₄ nanoparticles.     

Characterization and luminescence properties of Gd2O3 phosphor

Gd₂O₃ phosphor was synthesized by combustion synthesis using gadolinium nitrate hexahydrate as precursor and urea as fuel. Structural and surface morphology were studied by X-ray diffraction, transmission electron microscopy (TEM), and scanning electron microscopy (SEM). Chemical composition analysis of the phosphor was performed by Fourier-transform infrared spectroscopy, and tts optical properties were characterized by use of photoluminescence (PL) and thermoluminescence (TL) techniques. In PL spectra, feeble emission at 490 nm (blue) and intense emission at approximately 545 nm (green) are observed after excitation at 300 nm. TL measurement was performed on the Gd₂O₃ phosphor by irradiating it with γ-rays (1 kGy). A well resolved glow peak at 226.4 °C was observed. Kinetic data were estimated from the TL glow curve by use of Chen’s peak-shape method; the results are discussed in detail. The average particle size of the Gd₂O₃ phosphor was 41 nm; a monoclinic phase was formed at a firing temperature of 500 °C. This was in agreement with SEM and TEM results.     

Preparation of ZnFe2O4 Nanofibers by Sol‐Gel Related Electrospinning Method

Zinc ferrite gel fibers were prepared from the sol precursor by the electrospinning method, and the ZnFe₂O₄ polycrystalline nanofibers were obtained upon calcination of the gel fibers. The obtained ZnFe₂O₄ nanofibers composed of 20–30 nm nanocrystals were about one hundred to several hundred nanometers in diameter. The materials have been characterized by means of SEM, TEM, XRD, TGA, and IR techniques.     

Unexpected phase transformation from VO2(R) to VO2(A) during hydrothermal treatment in the V2O5�CH2C2O4�CH2O system

Vanadium dioxide (VO₂) was directly synthesized via the reduction of V₂O₅ with oxalic acid adopting two different types of hydrothermal processes in the temperature ranging from 180 to 260 °C. The products were characterized by X-ray diffraction, field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), and X-ray photoelectron spectroscopy (XPS). In all these processes, the VO₂(B) phase was first formed at a relative lower temperature or the initial stage at higher temperature and then it transformed to the VO₂(R) phase with the increase of temperature. The building-block-stacking mechanism was proposed to elucidate the transformation from VO₂(B) nano-plates to snowflake-like VO₂(R) powders. During this transformation, no trace of the VO₂(A) phase was observed when one-step hydrothermal treatment method was used, whereas some part of the branches of the snowflake-like VO₂(R) particles transformed to metastable VO₂(A) nanofibers in the autoclave during cooling process when the two-step hydrothermal treatment method was conducted. The reason for this transformation can be contributed to the defects formed during the stacking process.     

Catalytic activity of nanocrystalline ZnM2O4 (M = Fe,Co) prepared via simple and facile synthesis of thermal decomposition of mixed metal complexes of Schiff bases generated from α-ketobutyric acid and diaminoguanidine

Metal complexes ([ML₂], where M = Fe, Co, or Zn; HL = 2-[(6-ethyl-5-oxo-4,5-dihydro-2H-[1,2,4]triazin-3-ylidene)-hydrazono]-butyric acid, C₉H₁₃N₅O₃) of a Schiff base derived from α-ketobutyric acid (α-KBA) and diaminoguanidine (Damgu) were synthesized and characterized using elemental, spectral, and thermal studies. The metal complexes exhibited similar decomposition behavior, with a highly exothermic final decomposition step resulting in the formation of metal oxides. Isomorphism among the complexes was revealed using a powder X-ray diffraction (PXRD) technique. Solid solution precursors ([Zn_1/3M_2/3(L)₂], where M = Fe, Co) were synthesized and characterized using various physico-chemical techniques. A thermal decomposition technique was used to prepare spinel-type zinc cobaltite (ZnCo₂O₄) and zinc ferrite (ZnFe₂O₄) nanocrystalline particles with the synthesized single source precursors. Structural studies using PXRD ascertained the predominant crystal phase to be spinel. Transmission electron microscopy (TEM) and high-resolution TEM (HRTEM) showed a mean nanoparticle size of 18 ± 2 nm. Magnetic measurements revealed a weak magnetic behavior in the synthesized spinels. In the aqueous phase, the spinels exhibited catalytic activity, reducing 4-nitrophenol (4-NP) in the presence of NaBH₄ at room temperature. Additionally, the study demonstrated that the catalyst can be recovered and reused for five cycles with a more than 85% conversion efficiency.     

Superparamagnetic and ferromagnetic behavior of ZnFe2O4 nanoparticles synthesized by microwave-assisted hydrothermal method

Zinc ferrite (ZnFe₂O₄) nanoparticles were successfully synthesized from Zn(NO₃)₂ · 6H₂O and Fe(NO₃)₃ · 9H₂O by microwave hydrothermal method at 150°C for 1 h. Cubic ZnFe₂O₄ with particle size below 7 nm was formed in the solution at pH ≥ 6. The crystallinity and particle size of ZnFe₂O₄ nanoparticles were increased after calcination. The effects of pH of the precursor solution and calcination on the particle size and crystallinity of the particles were studied. At room temperature the products show superparamagnetic and ferromagnetic properties, determined by their size. The formation mechanism of ZnFe₂O₄ was also discussed according to the experimental results.

     

兼具电磁性能的PANI/ZnFe2O4纳米复合材料的制备

运用改进的溶胶凝胶-原位聚合法制备出了兼具电、磁性能的PANI/ZnFe2O4纳米复合材料,借助TEM、XRD、FTIR、四探针电导率仪和VSM(振动样品磁强计)等技术研究了复合材料的结构及其电磁性能。结果表明,通过该法可以实现ZnFe2O4与PANI的有机复合,制得纳米尺寸的、ZnFe2O4与PANI相间以化学键结合的纳米复合材料;复合材料兼具电、磁性能,其导电率随ZnFe2O4含量增加而降低,饱和磁化强度随之而升高,复合物的矫顽力在所研究的含量范围内均较纯ZnFe2O4大,且随ZnFe2O4含量的增加呈先升高后降低的变化趋势。此外,对ZnFe2O4进行HNO3预处理可以有效改善复合材料的电磁性能。     

Study of Microwave Torch Plasmachemical Synthesis of Iron Oxide Nanoparticles Focused on the Analysis of Phase Composition

This work presents the results obtained on the single-step route towards the synthesis of iron oxide nanoparticles in a microwave plasma torch. The torch is supplied by 660 sccm of Ar mixed with 1 sccm of Fe(CO)₅ and a variable amount of O₂. The influence of oxygen addition on the phase composition of the synthesized powder was studied. Magnetite and maghemite phases could not be distinguished using the standard X-ray diffraction (XRD) analysis. Therefore, a combined XRD and Raman spectra analysis had to be applied, which is based on fitting of selected diffraction peaks and spectral features. According to XRD and Raman spectroscopy, the powder synthesized from Ar/Fe(CO)₅ consisted about 50 % of magnetite, Fe₃O₄, the rest being α-Fe and FeO. An increase in oxygen flow rate led to an increase in γ-Fe₂O₃ percentage, at the expense of α-Fe, FeO and Fe₃O₄. Almost pure γ-Fe₂O₃ was synthesized at oxygen flow rates 25–75× higher than the flow rate of Fe(CO)₅. A further increase in the oxygen flow rate led to α-Fe₂O₃ and ε-Fe₂O₃ production. The distributions of nanoparticles’ (NPs) diameters were obtained using transmission electron microscopy (TEM) and dynamic light scattering (DLS). The mean diameter of the NPs measured by TEM was 13 nm while the DLS measurements led to the mean diameter of 12 nm. About 90 % of all particles had the diameter in the range of 5–21 nm but a few larger particles were observed in TEM micrographs.     

Synthesis and electrochemical characterization of duo doped spinels (zinc and praseodymium) for use in lithium rechargeable batteries

LiMn₂O₄ and LiZn_xPr_yMn_2?x?yO₄ (x = 0.10–0.24; y = 0.01–0.10) powders have been synthesized by sol–gel method using palmitic acid as chelating agent. The synthesized samples have been subjected to thermo gravimetric and differential thermal analysis, X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray analysis (EDAX). The sol–gel route bestows low calcination temperature, shorter heating time, high purity, good control over stoichiometry, small particle size, high surface area, good surface morphology and better homogeneity, The XRD patterns reveal high degree of crystallinity and better phase purity. SEM and TEM images exhibit nano-sized nature particles with good agglomeration. EDAX peaks of Zn, Pr, Mn and O have been confirmed in actual compositions of LiMn₂O₄ and LiZn_xPr_yMn_2?x?yO₄. Charge–discharge studies of pristine spinel LiMn₂O₄ heated at 850 °C delivers discharge capacity of 132 mA h g^?1 corresponding to columbic efficiency of 73 % during the first cycle. At the end of 10th cycles, it delivers maximum discharge capacity of 112 mA h g^?1 with columbic efficiency of 70 % and capacity fade of 0.15 mA h g^?1 cycle^?1 over the investigated 10 cycles. Inter alia, all dopants concentrations, LiZn_0.10Pr_0.10Mn_1.80O₄ exhibits the better cycling performance (1st cycle discharge capacity: 130 mA h g^?1 comparing to undoped spinel 132 mA h g^?1) corresponding to columbic efficiency of 73 % with capacity fade of 0.12 mA h g^?1 cycle^?1.     

Facile synthesis and properties of ZnFe2O4 and ZnFe2O4/polypyrrole core-shell nanoparticles

We demonstrated that ZnFe₂O₄/polypyrrole core-shell nanoparticles could be facilely synthesized via in situ chemical oxidative polymerization of pyrrole monomers on the surface of ZnFe₂O₄ nanoparticles. The shell thickness of core-shell nanoparticles could be easily controlled by adjusting the amount of pyrrole monomers. The phase structures, morphologies and properties of the as-prepared products were investigated by XRD, TEM, SEM, VSM, and FTIR spectra. Magnetic studies revealed that the saturation magnetization (M_s) and coercivity (H_c) of ZnFe₂O₄/PPy core-shell nanoparticles is 17.8 emu/g and 130 Oe, respectively. The electromagnetic characteristics of products showed that ZnFe₂O₄/PPy core-shell nanoparticles exhibit excellent microwave absorption performance than ZnFe₂O₄ nanoparticles, such as more powerful absorbing property and wider electromagnetic wave absorbing frequency band due to the proper matching of the permittivity and the permeability of ZnFe₂O₄/PPy core-shell nanoparticles.     

Nonstoichiometric Zn Ferrite and ZnFe<Subscript>2</Subscript>O<Subscript>4</Subscript>/Fe<Subscript>2</Subscript>O<Subscript>3</Subscript> Composite Spheres: Preparation,Magnetic Properties,and Chromium Removal

Monodisperse and porous nonstoichiometric Zn ferrite can be prepared by a solvothermal method. Such non-Zn ferrite was used to be the precursor for synthesis of ZnFe₂O₄/Fe₂O₃ composite via calcination at 600°C for 3 h in air. X-ray powder diffractometer (XRD) and Energy Dispersive Spectrometer (EDS) proved the nonstoichiometry of Zn ferrite synthesized by solvothermal method and the formation of ZnFe₂O₄/Fe₂O₃ composite via calcination. TEM image showed that non-Zn ferrite spheres with wormlike nanopore structure were made of primary nanocrystals. BET surface area of non-Zn ferrite was much higher than that of ZnFe₂O₄/Fe₂O₃ composite. Saturation magnetization of non-Zn ferrites was significantly higher than that of ZnFe₂O₄/Fe₂O₃ composites. Calcination of non-Zn ferrite resulted in the formation of large amount of non-magnetic Fe₂O₃,which caused a low magnetization of composite. Because of higher BET surface area and higher saturation magnetization, non-Zn ferrite presented better Cr⁶⁺ adsorption property than ZnFe₂O₄/Fe₂O₃ composites.     

One-pot hydrothermal synthesis of reduced graphene oxide/zinc ferrite nanohybrids and its catalytic activity on the thermal decomposition of ammonium perchlorate

Reduced graphene oxide/Zinc ferrite (rGO/ZnFe₂O₄) nanohybrids are successfully decorated on the surface of the rGO sheets through a simple, one-step hydrothermal method. ZnFe₂O₄ nanoparticles (NPs) are homogeneously anchored on the rGO sheets. The rGO/ZnFe₂O₄ hybrids are characterized by XRD, FT-IR, XPS, TEM, Raman, BET. The rGO/ZnFe₂O₄ hybrids demonstrate amazing catalytic activity on thermal decomposition of ammonium perchlorate (AP), which is better than that of bare ZnFe₂O₄ NPs. TG-DTA results indicate that the ZnFe₂O₄ NPs in the hybrids with increasing ratio (1%, 3%, 5%) could decrease the second decomposition temperature of AP by 42.7?°C, 55.0?°C, 68.1?°C, respectively, and reduce the apparent activation energy of AP from 160.2?kJ?mol^?1 to 103.8?kJ?mol^?1. This enhanced catalytic performance is mainly attributed to the synergistic effect of ZnFe₂O₄ NPs and rGO.     

Photocatalytic performance of combustion-synthesized β and γ-Ga2O3 in the degradation of 1,4-dioxane in aqueous solution

Nanostructures of β and γ-Ga₂O₃ were prepared by the solution combustion route using urea as fuel. The synthesized nano photocatalysts were characterized by use of XRD, FT-IR, BET, TEM, TGA–DTA, DRS, and Raman spectroscopy. XRD and TEM investigations confirmed the nanostructures; particle size was in the range 3–5 nm for γ-Ga₂O₃ and 40–50 nm for β-Ga₂O₃. The specific surface area of γ-Ga₂O₃ was 91 m² g^?1 and that of β-Ga₂O₃ was 24.3 m² g^?1. The polymorphs of gallium oxide were used as photocatalysts for decomposition of 1,000 mg/l 1,4-dioxane. More than 90 % of the 1,4-dioxane could be degraded in less than 180 min by use of 10 mg/l photocatalyst + 0.5 ml H₂O₂. The efficiency of photocatalytic degradation of 1,4-dioxane by the synthesized photocatalysts was compared with that of P-25 TiO₂ and followed the order γ-Ga₂O₃ ≥ β-Ga₂O₃ > P-25 TiO₂. The degradation was found to follow pseudo first-order kinetics.     

基于N-乙酰-L-半胱氨酸修饰的ZnFe2O4@SiO2纳米材料手性识别酪氨酸对映异构体

我们将N-乙酰-L-半胱氨酸（NALC）修饰于ZnFe₂O₄@SiO₂纳米材料表面,制备了一种新型的手性纳米复合物（ZnFe₂O₄@SiO₂-NALC）,该材料能够简便、快速及高选择性地识别手性酪氨酸（Tyr）对映体。利用X射线粉末衍射（XRD）、红外光谱（FT-IR）、能量色散X射线光谱（EDS）、扫描电子显微镜（SEM）、高分辨率透射电子显微镜（HRTEM）和振动样品磁力计（VSM）等一系列表征手段对首次合成出的ZnFe₂O₄@SiO₂-NALC进行测试表征,并将其应用于对手性识别领域的探究。实验结果表明,利用光谱技术（紫外-可见光谱和荧光光谱）,ZnFe₂O₄@SiO₂-NALC可对Tyr对映异构体进行手性识别。此外,我们进一步对Tyr浓度和pH值等实验参数进行了优化。     

Nanocluster polyoxomolybdate supported on natural zeolite: a green and recyclable catalyst for epoxidation of alkenes

A heterogeneous catalyst for epoxidation of alkenes has been synthesized by introducing polyoxomolybdate into a natural zeolite as a solid and green support. The prepared catalyst was characterized by FT-IR, inductively coupled plasma optical emission spectrometry (ICP-OES), powder X-ray diffraction (XRD), N₂ absorption–desorption, field emission scanning electron micrograph (FE-SEM) and transmission electron microscopy (TEM). The catalytic investigations disclosed that nanocluster polyoxomolybdate supported on the surface is an active and recyclable catalyst in liquid phase alkene epoxidation in dichloroethane at 80 °C.     

Magnetic retrievable Ag/AgBr/ZnFe2O4 photocatalyst for efficient removal of organic pollutant under visible light

In the present work, a visible-light-driven Ag/AgBr/ZnFe₂O₄ photocatalyst has been successfully synthesized via a deposition–precipitation and photoreduction method. The crystal structure, chemical composition, morphology and optical properties of the as-prepared nanocomposites were characterized by X-ray diffraction spectroscopy, X-ray photoelectron spectroscopy, scanning electron microscopy, high-resolution transmission electron microscopy, energy-dispersive X-ray spectroscope, UV–vis diffuse reflectance spectroscopy and photoluminescence. The photocatalytic activities of the Ag/AgBr/ZnFe₂O₄ nanocomposites were evaluated through the photodegradation of gaseous toluene and methyl orange (MO) under visible light. The results revealed that the as-prepared Ag/AgBr/ZnFe₂O₄ nanocomposite exhibited excellent photocatalytic activity. The degrading efficiency of MO could still reach 90% after four cycles, and the Ag/AgBr/ZnFe₂O₄ nanocomposite could be recycled easily by a magnet. Additionally, the enhanced photocatalytic mechanism was discussed according to the trapping experiments, which indicated that the photo-generated holes (h⁺) and •O₂⁻ played important roles in photodegradation process. At last, a possible photocatalytic oxidation pathways of toluene was proposed based on the results of GC–MS. The Ag/AgBr/ZnFe₂O₄ composites showed potential application for efficient removal of organic pollutant.     

Hydrogen production by methanol steam reforming on a cordierite monolith reactor coated with Cu–Ni/LaZnAlO<Subscript>4</Subscript> and Cu–Ni/γ-Al<Subscript>2</Subscript>O<Subscript>3</Subscript> catalysts

The performance of Cu–Ni/LaZnAlO₄ and Cu–Ni/γ-Al₂O₃ catalysts in the methanol reforming process in a monolith reactor in the temperature range of 200–350 °C, feed flow rate of WHSV = 20.8 h^?1 and atmospheric pressure has been investigated. In order to perform a more thorough investigation, surface area, morphology and crystalline structure of the synthetic catalysts have been studied using BET, FE-SEM, TPR, FT-IR, TEM, TGA and XRD analyses. The results have shown that Cu–Ni/LaZnAlO₄ catalyst synthesized by combustion reaction method under ultrasound irradiation has a very high efficiency and catalytic activity, low reduction temperature, high mechanical resistance and large pore sizes. The latter causes a higher percentage of active metal impregnation and better distribution on the support, greater resistance against sintering and maintenance of catalyst inertness at temperatures over 1000 °C, in comparison with conventional catalysts such as Cu–Ni/γ-Al₂O₃. This make its substitution for currently used catalysts affordable.     

Preparation and characterization of magnetic TiO2/ZnFe2O4 photocatalysts by a sol–gel method

A magnetic TiO₂/ZnFe₂O₄ photocatalyst was prepared by a sol-gel method, and X-ray diffraction (XRD), magnetic and photocatalytic properties analysis were employed to characterize this photocatalyst. The XRD results show that ZnFe₂O₄ can prevent the transformation of titania from anatase to rutile. The magnetic properties analysis indicates that TiO₂/ZnFe₂O₄ is of large saturation magnetization value and low coercivity. The photocatalytic experimental results show that TiO₂/ZnFe₂O₄=3 and 4 are superior in photocatalytic reactivity to other proportions. TEM shows that TiO₂/ZnFe₂O₄ has a fine core-shell fabric. After being used for four times during the photocatalytic reaction, the TiO₂/ZnFe₂O₄ nanoparticles have good photocatalytic stability.