流变相-前驱物法制备纳米镍铁氧体粉末

以乙酸镍、氢氧化铁和草酸为原料,用流变相反应法制备出前驱物,在不同温度下煅烧得到纳米镍铁氧体粉末。采用差热(TG-DSC)、X射线衍射(XRD)及透射电镜(TEM)对煅烧过程和产物进行了分析。结果表明,用流变相反应法制备的前驱物,在300℃煅烧即可直接形成纯相的尖晶石结构的镍铁氧体粉末。粉末呈方块状,平均颗粒大小约30 nm,分布均匀,分散性较好。相对其他方法,其煅烧温度低,可以克服因高温煅烧引起的颗粒增大和团聚的缺陷。     

Ni catalysts from NiAl2O4 spinel for CO2 reforming of methane

A series of mixed oxides close to NiAl₂O₄ was obtained by a sol–gel like method (propionic acid). The characterization of the different structures was made by X-ray diffraction (XRD), scanning electron microscopy (SEM) or transmission electron microscopy (TEM). For the stoichiometric ratio of Ni to Al exactly equal to 0.5, homogeneous crystalline spinel phase was formed for a temperature of calcination equal or higher than 725 °C. A solid solution was obtained for a Ni/Al ratio lower than 0.5. The spinel structure is non-tolerant concerning a change of nickel to aluminum ratio higher than 0.5: an excess of nickel gives large particles of NiO on spinel phase. Comparative reduction and dry reforming of these oxides was made to control the formation of Ni and its sintering for applications in methane dry reforming. Preliminary reactivity results in dry reforming of methane are given.     

Synthesis and characterization of monodisperse NiFe2O4 nanoparticles

Narrow size distribution nickel ferrite nanoparticles with average particle size of around 6 nm has been synthesized via rapid thermo-decomposition method in the presence of oleylamine in solution which acted as neutralizing, stabilizing and reducing agent OAm coated NiFe₂O₄ NPs. X-ray powder diffraction (XRD), Fourier Transform Infrared Spectra (FT-IR), Thermal Gravimetric Analysis (TGA), Scanning Electron Microscopy (SEM), Transmission electron microscopy (TEM), Vibrating Simple Magnetometer (VSM) and also Mössbauer Spectroscopy were used for structural, morphological, spectroscopic and magnetic characterization of the product. The XRD analysis revealed the formation of single phase nickel ferrite with Fd-3m space group. Both FT-IR and TGA analyses confirmed the formation of desired nanocomposite. FT-IR analysis also showed characteristic IR absorption bands of the spinel nickel ferrite phase and oleylamine. TEM and SEM analysis showed that product have almost spherical structural morphology. TEM images showed that NiFe₂O₄ nanoparticles have narrow size distribution and Energy Dispersive X-ray (EDX) analysis confirmed the presence of metal ions in the required stoichiometric ratio. Superparamagnetic property of the product was confirmed by VSM. From ⁵⁷Fe Mössbauer spectroscopy data, the variation in line width, isomer shift, quadrupole splitting and hyperfine magnetic field values have been determined. The Mössbauer spectra for OAm coated NiFe₂O₄ NPs. is consisting of one paramagnetic central doublets and one magnetic Zeeman sextet. Finally, the synthetic procedure can be extended to the preparation of high quality metal or alloy nanoparticles.     

Some new observations on the structural and phase evolution of nickel titanate nanofibers

In this study, we report for the first time the synthesis of nickel titanate (NTO) nanofibers containing a mixture of ilmenite and spinel phases of NTO, at an atypical low temperature. Precursor nanofibers produced by sol-gel electrospinning were calcined at three different temperatures to produce the NTO nanofibers. Thermal analysis along with X-ray photoelectron spectroscopy confirmed the formation of non-crystalline stable phases of TiN and Ti-O-N that restrained the formation of ilmenite NTO, and the Ni-rich environment pushed the Ti atoms to tetrahedral sites to form a defective spinel structure. The crystallite size of spinel NTO was observed to increase as a function of the calcination temperature above 700 °C, as the activation energy for coalescence and growth of spinel NTO was favorable. NTO nanofibers obtained above the calcination temperature of 700 °C exhibited new band gap energy around 2.5 eV in Tauc plot. Oxygen vacancies in these ceramic nanofibers decreased as the calcination temperature was increased. A hypsochromic shift of 20 nm in the photoluminescence spectra suggested that the material had a Ni²⁺ rich NTO (spinel).     

Simplified synthesis of isomorphously nickel substituted ZSM-5

Isomorphously nickel-substituted nano-crystalline ZSM-5 is synthesized in the absence of acidic aqueous fluoride medium incorporating simple and low-cost metal inorganic salt precursor NiCl₂.6H₂O instead of large organic cationic salt like bis (tetraethyl ammonium) tetrachloronickelate (II) with less water quantity to minimize the synthesis waste. PXRD, FT-IR, TG/DTG, XPS, UV–Vis DRS, SEM, TEM, ICP and N₂ adsorption-desorption techniques were used to confirm the presence of nano-crystalline material having a MFI structure and heteroatom substitution. The unit cell dimensions increase with increasing levels of nickel substitution. The crystallite size of as synthesized samples was in the range of 60–75 nm, which increased to 60–160 nm after calcination at 550°C. Percentage crystallinity and crystallite size increases with increasing nickel substitution level up to 0.17 mol and beyond that the material becomes amorphous.     

Nanocrystalline/Nanosized Ni1−γFe2+γO4 Ferrite Obtained by Contamination with Fe During Milling of NiO–Fe2O3 Mixture. Structural and Magnetic Characterization

The nanocrystalline nickel ferrite (NiFe₂O₄) was synthesized by reactive milling starting from equimolar mixture of oxides. The iron contamination during milling leads to a solid state reaction between Fe and NiFe₂O₄ spinel. This reaction starts for a milling time longer than 30 h. A mixed nickel–iron ferrite (Ni_1?γFe_2+γO₄) and elemental Ni are obtained. The evolution of the nickel–iron mixed ferrite during milling and its properties were investigated using X‐ray diffraction, Fourier Transform Infrared Spectroscopy (FTIR), Laser Particles Size Analyzer and magnetic measurements. Annealing treatment (350°C/4 h in vacuum) is favorable to the reaction between phases. Replacement of Ni²⁺ cations by iron cations provided by contamination leads to the increase of lattice parameter value of the spinel structure. The magnetization of the nickel–iron mixed ferrite newly formed is larger than the nickel ferrite magnetization (13.6 μ_B/f.u. and 6.22 μ_B/f.u., respectively), due to the magnetic moment of Fe²⁺ cation which is double as compared to the Ni²⁺ cation. Magnetization of the milled samples decreases during milling due to the structural changes induced by milling in the nickel–iron mixed ferrite. The annealing induces a reordering of the cations which leads to a larger magnetization.     

The catalytic activity of Ni/W bimetallic sulfide nanostructured catalysts in the hydrodesulfurization of dibenzothiophene

Two types of catalysts containing NiW bimetallic sulfide nanostructures were prepared by a chemical method employing ammonium thiotungstate and nickel nitrate as metal-sulfide precursors followed by sulfidation in H₂S/H₂ at 400 °C. The nanostructures were grown with excess of Ni, at atomic ratio R = 0.75, 0.85 (R = Ni/Ni + W). High resolution electron microscopy (HRTEM) micrographs revealed the formation of two types of nanostructures, nickel sulfide nanoparticles and long nanorods of tungsten suboxide, both coated by WS₂ layers. The Ni/W catalyst containing mostly nanorods presented twice the catalytic activity (pseudo-zero order constant rate k = 12 × 10⁻⁷ mol/s.g) of the Ni/W catalyst containing nanoparticles (k = 6.3 × 10⁻⁷ mol/s.g) with a low selectivity for tetrahydrodibenzothiophene (THDBT) and high selectivity to cyclohexylbenzene (CHB, 50 mol%). In turn the Ni/W catalyst containing nanoparticles presented a catalytic activity comparable to a Ni/Mo catalyst without inorganic fullerene (IF) nanostructures (k = 7.2 × 10⁻⁷ mol/s.g) but with higher selectivity for hydrogenation to THDBT, (14 mol%) than the sample with nanorods.     

Oxygen Content of Nickel Ferrites at 1300°C

The oxygen contents for compositions with the spinel structure in the system Fe-Ni-O were determined at 13OO°C for oxygen pressures from 10^−3.6 to 10°atm. The ferrite region, from an Fe/Ni ratio of 2.035 to magnetite, was investigated. Below Fe/Ni = 2.5 only oxygen-deficient ferrites exist. Above Fe/Ni = 7.6 only ferrites with an oxygen excess were found and for the intermediate nickel contents, ferrites with both types of oxygen nonstoichiometry were found. Previous phase equilibria studies, which do not report single-phase ferrite with an oxygen deficiency, are discussed.     

Graphene anchored Ce doped spinel ferrites for practical and technological applications

Graphene plays a remarkable role as a supporting material for the fabrication of a variety of nanocomposites. This work presents the fabrication of graphene-based Ce doped Ni–Co (Ni_0.5Co_0.5Ce_0.2Fe_1.8O₄/G) ferrite nanocomposites. Ni_0.5Co_0.5Fe₂O₄ and Ni_0.5Co_0.5Ce_0.2Fe_1.8O₄ were prepared using sol gel method. However, Ce doped Ni–Co spinel nanoferrite was chemically anchored on the surface of graphene. Different characterizations techniques were adopted to investigate the variations in the properties of ferrite composite due to the incorporation of graphene. Thermal analysis revealed 18% heat weight loss of Ce doped Ni–Co ferrite sample during treatment up to 1000 °C respectively. X-ray diffraction analysis depicted the presence of spinel phase structure of all synthesized nanocomposites. Fourier transform infrared analysis revealed two absorption bands of tetrahedral and octahedral sites of the spinel phase and presence of graphene contents in the Ni_0.8Ce_0.2CoFeO₄/G composite. FESEM images revealed an increased agglomeration due to the presence of graphene in the Ce doped Ni–Co ferrite composites. Graphene based Ce doped Ni–Co ferrite nanocomposite showed highest conductivity (4.52 mS/cm) than other ferrite composites. Magnetic characteristics showed an improvement in the Ni–Co ferrite sample by the substitutions of Ce³⁺ ions and graphene contents. The improvement in the properties of these nanocomposites makes them potential material for many applications such as fabrication of electrodes, energy storage and nanoelectronics devices.     

Facile synthesis of metal-doped Ni-Zn ferrite from treated Zn-containing electric arc furnace dust

Metal-doped Ni-Zn ferrite with a spinel structure was directly synthesized from treated zinc-containing electric arc furnace dust (Zn-containing EAFD) by solid state reaction method, realizing the transformation of solid waste to high value-added material. First, NiCl₂·6H₂O was added to the treated Zn-containing EAFD before calcination. Then, the effects of the mass ratio of treated Zn-containing EAFD to NiCl₂·6H₂O (R_TZE/N, g g⁻¹) and the calcination temperature on the synthesis and magnetic properties of as-synthesized samples were systematically investigated by X-ray diffraction, Raman spectroscopy and physical property measurement. It was found that R_TZE/N and calcination temperature significantly influenced the synthesis of single-phase spinel ferrite and their magnetic properties. Pure metal-doped Ni-Zn ferrite, exhibiting good magnetic properties of higher saturation magnetization (Ms, 60.5 emu g⁻¹) and lower coercivity (Hc, 49.8 Oe), was obtained when the calcination temperature was controlled at 1100 °C for 2 h with a R_TZE/N of 1:0.9.     

Corrosion of nickel ferrite refractory by Na3AlF6–AlF3–CaF2–Al2O3 bath

Based on research on cermet inert anodes for aluminium production, it has been suggested that nickel ferrite spinel might be suitable for use as a sidewall refractory in Hall-Héroult cells. A corrosion resistant sidewall would allow elimination of the frozen bath ledge, and has potentially huge benefits in terms of energy savings and increased productivity. However, little work has been done to assess nickel ferrite's suitability as a refractory.Dense nickel ferrite samples were prepared and characterized, and corrosion tests in cryolite based baths were conducted. Results confirm that the spinel does have good corrosion resistance. The corrosion mechanism is complex, involving grain boundary attack and formation of a Ni–Fe alloy. This alloy could pose a risk in terms of contamination of the aluminium. The use of additives to restrict penetration of grain boundaries may be the key to development of a successful spinel based refractory.     

Combustion synthesis of nanocrystalline nickel ferrite using hexamine as a fuel

Nanocrystalline nickel ferrite has been synthesized by novel combustion method using hexamine as a fuel and metal nitrates as oxidizers. The prepared compounds were sintered at 750°C. The synthesized ferrite powders were characterized by XRD, FTIR, EDAX, and SEM. XRD data confirm the formation of single-phase spinel nickel ferrite compound. FTIR spectra show the stretching and bending vibrations of Ni-O and Fe-O bonds in nickel ferrite. The elemental composition of the synthesized compound was assessed by EDAX analysis. The morphological features of the ferrite powders were scrutinized by SEM.     

Thiophene hydrodesulfurization using unsupported nickel-neodymium bimetal catalysts

The hydrodesulfurization of thiophene was studied over unsupported nickel-neodymium bimetallic catalysts. The physical and chemical changes of bimetals were observed after calcination and presulfidation, respectively. The activity was increased with addition of neodymium to nickel catalysts and was in good correlation with the surface area of catalysts. Qualitative evidence from XRD and SEM on the role of Nd as a structural promoter were provided.     

MIL-53(Fe)金属有机骨架材料对刚果红的高效吸附

通过水热法制备规则外形的MIL-53(Fe)金属有机骨架材料(MOF),并通过傅里叶红外光谱(FT-IR)、X射线衍射(XRD)、扫描电镜(SEM)和透射电镜(TEM)对材料进行表征。以刚果红作为目标物,研究所制得的MOF材料对其的吸附行为。结果表明,MIL-53(Fe)对刚果红的吸附动力学符合准二级动力学,吸附模型符合Langmuir吸附模型。MIL-53(Fe)材料对刚果红的最大吸附量为1 482 mg/g,是可望用于去除染料废水刚果红的高效吸附材料。     

Phytoextract assisted hydrothermal synthesis of ZnO–NiO nanocomposites using neem leaves extract

This work represents the synthesis of zinc oxide nanorods, nickel oxide nanoparticles, and zinc oxide-nickel oxide nanocomposites by combining Neem leave extract with hydrothermal synthesis. Five samples were prepared by green synthesis which is based on Neem leaves aqueous extract followed by hydrothermal treatment at 250 °C for 2.5 h. The five prepared samples are: 100% NiO (N100), 75% NiO: 25% ZnO (Z25-N75), 50% NiO: 50% ZnO (Z50-N50), 25% NiO: 75% ZnO (Z75-N25), and 100% ZnO (Z100). The prepared nanoparticles and nanocomposites were characterized by FTIR, XRD, SEM, and TEM. The XRD results show that the ZnO formed as a hexagonal wurtzite phase and NiO as a cubic phase. The microstructure of the formed samples is versatile with nanorods ZnO and spherical NiO. The nanocomposites microstructure appears as a heterostructure of both oxides with NiO particles on the surface of ZnO rods. The TEM confirms the nanosize and the crystallinity of samples.     

Nanostructured nickel ferrite: A liquid petroleum gas sensor

The present investigation deals with the synthesis of nanostructured nickel ferrite (NiFe₂O₄) and their liquid petroleum gas-sensing characteristics. The 15–20 nm size nickel ferrite has been synthesized at 700 °C by a simple molten-salt route using sodium chloride as grain growth inhibitor. These nanoparticles exhibit significantly high response towards liquid petroleum gas (LPG) in comparison with ethanol vapor, hydrogen sulfide, ammonia and hydrogen. The gas response towards various gases at their 200 ppm concentrations is investigated at 200–450 °C. Different characterization techniques have been employed, such as differential thermal analysis, X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and high resolution transmission electron microscopy (HRTEM) to study the crystallite size, structure and morphology. The results suggest possibility of utilization of the nanostructured nickel ferrite, without addition of any precious metal ion, as the LPG detector.     

Ni–Fe mixed oxides prepared by calcination of layered double hydroxides: Potential pigments for the ceramic industry

Mixed Ni,Fe oxides have been prepared by calcination of precursors with the hydrotalcite-type structure which had been prepared by the reverse micelle method using different surfactants. The solids have been characterized by several physicochemical techniques: Powder X-ray diffraction, nitrogen adsorption–desorption at −196 °C for specific surface area assessment, particle size distribution, UV–vis spectroscopy, and temperature-programmed reduction. The solids are formed by NiO and NiFe₂O₄ (spinel) and their properties depend on the experimental conditions used to prepare the hydrotalcite-type precursor. The crystallite size is larger for the spinel crystallites than for the NiO crystallites and in all cases depends on the surfactant used and the pH during the synthesis. The original, uncalcined samples, show intense mainly yellow color, but on calcination almost all of them change to dark brown or even almost black; only when using a cyclic surfactant the color is markedly different from that obtained when linear surfactants are used.     

柠檬酸盐凝胶的自燃烧与铁氧体纳米粉合成

借助差热分析、红外吸收光谱和Ｘ射线衍射技术研究了硝酸盐－柠檬酸盐凝胶的热分解和燃烧过程,发现具有一定组成的镍铜锌铁硝酸盐和柠檬形成的凝胶具有自蔓延燃烧特征,燃烧后直接形成粒径为２０～５０ｎｍ具有尖晶石结构的单相铁氧体粉末,调整硝酸盐和柠檬本的比例可控燃烧速率和燃烧过程,进而调控纳米粉末的颗粒尺寸和磁相结构。     

Synthesis of (Ni,Mn,Co)O4 nanopowder with single cubic spinel phase via combustion method

(Ni,Mn,Co)O₄ nanopowders with single cubic phase were successfully synthesized using combustion methods. Particle size of the as-burnt nanopowders after combustion was about 20 nm. Crystallization behavior of the NMC was investigated using various techniques such as X-ray diffraction (XRD), thermogravimetric (TG), Fourier transform infrared (FT-IR) spectroscopy, and transmission electron microscopy (TEM). Calcination at different temperature from 400 °C to 700 °C provides the powders with increased crystallinity and grain size. However, further increasing temperature above 800 °C for calcination, cubic spinel phase of NMC partly transformed to tetragonal spinel phase, which implies that cubic spinel phase of NMC nanopowder synthesized by combustion method becomes unstable above 800 °C.     

掺杂MnO2对铁酸镍陶瓷惰性阳极性能的影响

为了提高铝电解惰性阳极材料的性能,尝试在合成铁酸镍陶瓷阳极的过程中掺杂一定量MnO2. 采用高温固相反应法在1200℃下烧结6 h,制备了掺杂MnO2的铁酸镍阳极材料. 对掺杂试样进行X射线衍射分析,并且研究了掺杂MnO2对材料密度、导电性及抗弯强度和抗热震性的影响. 研究结果表明,掺杂MnO2后未形成新相,MnO2与NiFe2O4形成固溶体,Mn4+离子取代了部分Fe3+离子,材料仍是镍铁尖晶石结构;掺杂MnO2后,NiFe2O4的晶格产生畸变,说明MnO2促进了烧结,提高了材料的密度;并且由于Mn4+离子取代Fe3+离子,产生阳离子空位,改善了铁酸镍阳极的导电性. 同时MnO2对改善试样的抗弯强度及抗热震性也有明显作用.