Microwave-assisted synthesis of α-Fe2O3/ZnFe2O4/ZnO ternary hybrid nanostructures for photocatalytic applications

Solar-driven highly efficient photocatalytic decomposition of toxic organic contaminants using magnetically separable α-Fe₂O₃/ZnFe₂O₄/ZnO ternary hybrid nanodiscs is reported. α-Fe₂O₃/ZnFe₂O₄/ZnO ternary hybrid nanostructures were synthesized by microwave-assisted co-precipitation and simple co-precipitation methods and well characterized by XRD, micro-Raman, FESEM and UV–vis spectroscopy. FESEM micrographs revealed nanodiscs in case of microwave-assisted co-precipitation whereas nanoparticles and their aggregates were formed under co-precipitation combined with calcination. XRD and Raman studies confirmed the hybrid nature of prepared α-Fe₂O₃/ZnFe₂O₄/ZnO nanostructures. Photocatalytic performance of α-Fe₂O₃/ZnFe₂O₄/ZnO hybrid nanostructures was investigated by carrying out the photodegradation of organic dyes MB and MG under solar light illumination. The prepared α-Fe₂O₃/ZnFe₂O₄/ZnO ternary hybrid magnetic nanodiscs decomposed MB and MG dyes in only 32 and 24 min, respectively. α-Fe₂O₃/ZnFe₂O₄/ZnO hybrid nanodiscs showed excellent photocatalytic performance together with reusability and easy magnetic separation demonstrating its suitability for solar-driven photocatalytic water purification applications. In-situ scavenger studies showed ?OH radicals are the main active radicals in solar-driven photocatalysis by α-Fe₂O₃/ZnFe₂O₄/ZnO nanodiscs. The tentative mechanism of growth of α-Fe₂O₃/ZnFe₂O₄/ZnO ternary hybrid nanodiscs and the photocatalytic mechanism are discussed.     

Hydrothermal synthesis and characterization studies of α-Fe2O3/MnO2 nanocomposites for energy storage supercapacitor application

In this present study, semiconductor magnetic α-Fe₂O₃/MnO₂ nanocomposites (NCs) were prepared by a facile hydrothermal (HT) method. The crystallographic structure, morphology, chemical configuration and magnetic features were analysed by X-ray powder diffraction (XRD), high resolution scanning electron microscope (HR-SEM), energy dispersive X-ray analysis (EDX), transmission electron microscope (TEM), Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS) and vibrating sample magnetometer (VSM) analyses. The as-prepared NCs were used as an electrode in energy storing supercapacitor was systematically examined. The electrochemical deeds of α-Fe₂O₃/MnO₂ NCs was analysed by cyclic voltammetry (C–V) and galvanostatic charge–discharge (GCD) tests. The CV analysis of the NCs electrode showed a distinctive pseudocapacitive behaviour in 1 M KOH solution. The NCs electrode reveals enhanced specific capacitance compared to plain α-Fe₂O₃ and MnO₂ nanoparticles (NPs) and generates high specific capacitance of 216.35 Fg⁻¹. Pseudocapacitor obtains of energy density 135.42 Wh kg⁻¹ at power density of 6.399 kW kg⁻¹, indicating the as-prepared α-Fe₂O₃/MnO₂ NCs shows noteworthy high-energy, specific capacitance, power densities and long-standing cyclic stability with 89.2% of preliminary capacitance reserved at 1A g⁻¹ after 10000 cycles in judgement with the pure α-Fe₂O₃ and MnO₂ NPs electrode. The α-Fe₂O₃/MnO₂ NCs electrode having noteworthy electrochemical characteristics performance renders promising applications in energy storing systems.     

Mechanochemical synthesis of α-Al2O3-Cr3+ (Ruby) and χ-Al2O3

In this work we present a unique method to synthesize χ-Al₂O₃ and α-Al₂O₃ doped with Cr³⁺ (ruby). The ruby is synthesized by mechanical milling of pseudoboehmite that is doped in-situ with chromium. The doping is carried by adding chromium sulfate hydrate to an aqueous solution rich in aluminum sulfate hydrate. The pH in the solution is controlled to be between 9 and 10 by using ammonia, which induces the pseudoboehmite precipitation. The Cr³⁺ is added for its remarkable effects on the detectability of ruby emitting luminescent R₁ and R₂ bands that are traceable in Raman spectroscopy. The formation of ruby is detected at milling times as short as 5 hours and increased with the milling time. Ruby phase is further confirmed by means of true atomic resolution Transmission Electron Microscopy (TEM).     

Novel synthesis and characterization of nanosized γ-Al2O3 from kaolin

This paper reports the synthesis of nanosized γ-Al₂O₃ from acid-leachates of calcined kaolin. Al (hydr)oxide was precipitated with ammonia from the leachate in the presence of polyethylene glycol. A white powder of nanosized γ-Al₂O₃ particles was obtained after calcination. X-ray diffraction (XRD), different scanning calorimetries and thermogravimetry (DSC-TG), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR) and magic angle spinning nuclear magnetic resonance (MAS NMR) were used to characterize the samples. Typical nanosized γ-Al₂O₃ particles showed rod-like morphology with width of about 7 nm and length of approximately 20 nm. A possible mechanism from kaolin to nanosized γ-Al₂O₃ is proposed.     

Hydrothermal synthesis and visible-light photocatalytic activity of α-Fe2O3/TiO2 composite hollow microspheres

Novel α-Fe₂O₃/TiO₂ composite hollow spheres were successfully synthesized by a template-assisted precipitation reaction using urea as a precipitating agent and carbon spheres as templates in a mixed solvent of water and ethanol, and then calcined at 400 °C for 4 h. The as-prepared samples were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, nitrogen adsorption–desorption isotherms, and vibrating sample magnetometer. The influence of calcination temperature and the molar ratio of titanium to iron (R) on the photocatalytic activity of the samples was investigated. The results indicated that the composite spheres show magnetic characteristics at room temperature and good photocatalytic activity under visible-light irradiation compare to the single-component α-Fe₂O₃ particles. This method can be further applied to synthesize nanocomposites of magnetic metal oxide and other metal oxide.     

Phase metastability of nanosized α-Al2O3 crystallites

The reversal of the α- to θ-Al₂O₃ phase transformation and the induced microstructure evolution of boehmite-derived discrete nanosized α-crystallites are examined. Three categories of α-crystallites smaller than 100 nm were examined and found to have similar behavior: (1) pre-existing α-crystallites, (2) α-crystallites formed in situ during the calcination of θ-crystallites of sizes near the critical size, 25 nm, and (3) α-crystallites formed in situ by the thermal treatment of as-received θ-crystallites. The α-crystallite may transform back to the θ-phase above 800 °C. The backwards θ-crystallite may also re-transform to the α-phase again. Because of the density difference between α- and θ-Al₂O₃, the strain involved in the volume expansion and shrinkage during the phase transition eventually results in the formation of a twinned and/or mosaic structure for the θ- and α-crystallites. A strain release model representing the microstructure evolution of the α- to θ-phase and the θ- to α-Al₂O₃ phase transformation is proposed.     

Hydrothermal synthesis, crystal structure and properties of complex [Co (odpa) (phen) 2 ( H2O )] · H2O

以4,4’-氧化二苯四羧酸二酐和1,10-邻菲啰啉为配体在水热条件下合成了标题配合物,并用元素分析、红外光谱、X-射线单晶衍射以及热重分析对配合物进行了表征.晶体结构分析表明配合物为三斜晶系,P-1空间群a=11.190(2)(A),b=12.587(2) (A),c=13.097(3)(A),α=102.688(3)°,β=105.751(2)°,γ =92.615(2)°,V =1721.1(6)A3,Z=2.配合物为单核结构,相邻的单核分子通过氢键的识别作用形成一维超分子双链.π…π堆积作用和C-H…π之间弱相互作用将邻近超分子双链的进一步扩展为三维超分子结构.     

Simultaneous control of particle size and morphology of α-CaSO4·1/2H2O with organic additives

Here we reported a method to simultaneously control the particle size and morphology of α-CaSO₄·1/2H₂O (α-HH) prepared from flue gas desulfurization gypsum by adjusting the succinic acid concentration and glycerol content under mild conditions. Succinic acid controlled the crystal morphology by adsorption onto α-HH surfaces, and glycerol controlled the crystal particle size, in which an increase in the maximal relative supersaturation (S_max) and nucleation rate of α-HH was hypothesized to cause the change in α-HH particle size. Then, based on the method, α-HH with different particle sizes but with almost the same morphology was prepared, and the influence of the crystal particle size on the mechanical strength of the α-HH pastes was explored. With decreasing α-HH particle size from about 26 to 5 μm, the dry compressive strength of the pastes made from the α-HH decreased remarkably from 68.02 to 34.85 MPa, which was ascribed to an increase in the internal porosity of the pastes.     

Nd(OH)3-Co3O4-Nb2O5纳米复合掺杂BaTiO3基陶瓷研究

钛酸钡(BaTiO3)材料具有铁电、压电、热电、介电等特性,广泛用于制造高介电容器、热敏电阻和换能器等,特别是用作多层陶瓷电容器(MLCC)的基质材料.目前,MLCC向高可靠性、高比容(小尺寸大容量)、低成本的趋势发展.因此,制备高纯超细的BaTiO3粉体以及掺杂改性的研究,是该领域研究的热点.本文制备了Nd(OH)3...     

Effect of citrate to nitrate ratio on the sol-gel synthesis of nanosized α-Al2O3 powder

This paper studied the effect of the variation of citrate to nitrate ratio on the sol-gel synthesis of nanocrystalline α-alumina powder. The process involves the formation of a sol using aluminium nitrate and citric acid which then transferred to a transparent gel and finally to a powdery mass. The prepared alumina powder was thoroughly characterised by different techniques such as phase analysis, thermal analysis, microstructure study, etc. Variation in citrate to nitrate molar ratio (C/N) influenced the thermal decomposition behaviour, particle size distribution, phase transformation temperature and specific surface area of the developed powder. The complete formation of α- Al₂O₃ was obtained at around 950 °C for C/N=1.5. The unimodal distribution of the particles within a narrow size range and higher particle to particle linking through solid bridging are the characteristics of the powder prepared at C/N=1.5. It was found higher citrate to nitrate ratio in the fuel rich condition is responsible for better properties of synthesised alumina powder.     

(Bi13Co11)Co2O40–Co3O4 nanocomposites: Synthesis,characterization and application as substrate for microstrip patch antenna

The sillenite-cobaltite nanocomposites with chemical formula (Bi₁₃Co₁₁)Co₂O₄₀–Co₃O₄ were synthetized and characterized for application as substrate in a microstrip patch antenna. To prepare the sample, the combustion method using urea as fuel was applied. The structural and vibrational characterizations were done through X-ray diffraction and infrared spectroscopy. The morphology of the sample was studied through FESEM images. The magnetization as a function of magnetic field recorded at 300 K confirmed the paramagnetic character of the sample. Electric characterization was performed from 1.0 GHz to 8.5 GHz aiming a wide frequency spectrum data, presenting steady real relative permittivity around 7, with low losses as results. A microstrip patch antenna was designed by cavity method with the nanocomposite as substrate for application in X-band communication services. Reflection coefficient measurements displayed a good agreement with simulations, achieving only 0.39% error in resonance frequency, validating the performed morphological and electrical characterizations, as antenna design. Simulated radiation pattern is also presented, with coherent results for a directive device.     

Facile synthesis of morphology and size-controlled α-Fe2O3 and Fe3O4 nano-and microstructures by hydrothermal/solvothermal process: The roles of reaction medium and urea dose

This paper reports a systematic study of the influences on the synthesis of α-Fe₂O₃ and Fe₃O₄ via a hydro/solvothermal process at 200 °C. Both the reaction medium and urea dose have been investigated. The products were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), transmission electron microscopy (TEM). Results showed that the reaction mediums, such as water and ethylene glycol, played important roles in forming different types of iron oxides. Pure crystalline α-Fe₂O₃ was formed via the hydrothermal process, and Fe₃O₄ was obtained through a solvothermal route with ethylene glycol as reaction medium. Increasing urea dose tuned the particle sizes of α-Fe₂O₃ and Fe₃O₄ from a few hundreds to several tens of nanometers. With addition of urea, the morphology of α-Fe₂O₃ evolved from olive-like to rhomb-like, and Fe₃O₄ evolved from hollow sphere, to pinecone-like, and finally into cracked nanostructures. The variations of the surface area of products were mainly dependent on the microstructure and intrinsic features of the iron oxide particles. Results of the mechanistic studies indicated that the generation of CO₂ and NH₃ via in situ thermal decomposition of urea was crucial for the formation of α-Fe₂O₃ and Fe₃O₄ nano-and microstructures. The as-synthesized α-Fe₂O₃ and Fe₃O₄ were used as catalysts for methylene blue degradation in the presence of H₂O₂, and α-Fe₂O₃ showed a higher degradation efficiency. Our findings demonstrated a promising strategy for the developments of rationally designed iron oxides.     

Hydrothermal solvothermal synthesis and microwave absorbing study of MCo2O4 (M = Mn,Ni) microparticles

ABSTRACT

MCo₂O₄ (M?=?Mn,Ni) microparticles were synthesised by a simple hydrothermal solvothermal method. The samples were characterised by X-ray diffraction, X-ray energy dispersive spectroscopy and scanning electron microscopy, which showed that MnCo₂O₄ microparticles with spherical particles aggregated by a large number of small cubes and cubic shaped NiCo₂O₄ microcubes were obtained. The microwave absorption properties of these products were systematically investigated by vector network analysis. Results indicated that the minimum reflection loss value of MnCo₂O₄ microparticles was ?26.34?dB at 11.04?GHz with the absorber thickness of 2.5?mm, which was much lower than that of NiCo₂O₄ microcubes with the same absorber thickness. The possible mechanism was analysed, indicating that the geometry and size of MCo₂O₄ (M?=?Mn,Ni) microparticles played a key role in microwave absorption.     

High-pressure behavior and phase stability of Na2B4O6(OH)2·3H2O (kernite)

The high-pressure behavior of kernite [ideally Na₂B₄O₆(OH)₂·3H₂O, a ~ 7.02 Å, b ~ 9.16 Å, c ~ 15.68 Å, β = 108.9°, Sp Gr P2₁/c, at ambient conditions], an important B-bearing raw material (with B₂O₃ ≈ 51 wt%) and a potential B-rich aggregate in radiation shielding materials, has been studied by single-crystal synchrotron X-ray diffraction up to 14.6 GPa. Kernite undergoes an iso-symmetric phase transition at 1.6-2.0 GPa (to kernite-II). Between 6.6-7.5 GPa, kernite undergoes a second phase transition, possibly iso-symmetric in character (to kernite-III). The crystal structure of kernite-II was solved and refined. The isothermal bulk modulus (K_V0 = β^-1_P0,T0, where β_P0,T0 is the volume compressibility coefficient) of the ambient-pressure polymorph of kernite was found to be K_V0 = 29(1) GPa and a marked anisotropic compressional pattern, with K(a)₀: K(b)₀: K(c)₀~1:3:1.5., was observed. In kernite-II, the K_V0 increases to 43.3(9) GPa and the anisotropic compressional pattern increases pronouncedly. The mechanisms, at the atomic scale, which govern the structure deformation, have been described.     

One-step hydrothermal synthesis of hybrid core-shell Co3O4@SnO2–SnO for supercapacitor electrodes

We successfully synthesized a novel core-shell hybrid metal oxide via a simple one-step hydrothermal method without annealing. This composite of Co₃O₄ particles covered with SnO₂–SnO (Co₃O₄@SnO₂–SnO) predicted better performance compared to pure Co₃O₄, which strongly depends on the synthetic temperature. The Co₃O₄@SnO₂–SnO prepared at a temperature of 250 °C (labeled Co₃O₄@SnO₂–SnO-250) exhibited an outstanding specific capacitance of 325 F g⁻¹ under the current density of 1 A g⁻¹, which was much higher than those of Co₃O₄ (12.6 F g⁻¹) and other composites. Additionally, the sample also exhibited good cycle stability performance with a retention rate of 100% after 5000 cycles at a current density of 5 A g⁻¹. Through X-ray photoelectron spectroscopy analysis, the presumed mechanism was that Sn-O_x decreases the surface electron densities of Co₃O₄, which is beneficial to OH⁻ adsorption and specific capacitance improvement, and the synthetic temperature had a strong impact on the microstructure and thus on the surface electron densities. The most.obvious finding to emerge from this study is that the specific capacitance can be improved through adjusting the surface electron densities of transition metal oxides.     

Mechanochemical-molten salt synthesis of α-Al2O3 platelets

The polyaluminium chloride (PACl) precursor was used for a simple and scaled-up mechanochemical-molten salt synthesis of α-Al₂O₃ platelets. PACl, as a low temperature α-Al₂O₃ precursor, was firstly mechanically activated by high-energy ball milling for 5 min, followed by a next 5 min ball milling in the presence of a NaCl–KCl salt mixture. The starting formation temperature of the α-Al₂O₃ phase was 600 °C. In the subsequent annealing in the temperature range of 660–1000 °C, the α-Al₂O₃ phase with a well developed plate-like morphology was obtained. The products were characterized by X-ray powder diffractometry, scanning electron microscopy (SEM), and thermal analysis (DTA, TG) and solution ²⁷Al NMR spectroscopy.     

Preparation and electrochemical performances of doughnut-like Ni(OH)₂-Co(OH)₂ composites as pseudocapacitor materials

Doughnut-like nanostructured Ni(OH)(2)-Co(OH)(2) composites were prepared by combining hydrothermal and chemical deposition routes. The electrochemical performances of the composites were investigated as pseudocapacitor materials through galvanostatic charge-discharge and cyclic voltammetry tests. The Ni(OH)(2)-Co(OH)(2) composites delivered a specific capacitance of 2193 F g(-1) at 2 A g(-1) and 1398 F g(-1) at 20 A g(-1), much higher than those of pristine Ni(OH)(2). The enhancement of the overall electrochemical performances is ascribed to the synergetic contribution from nanostructured Ni(OH)(2) and electrically conductive CoOOH forming in the charge process.     

Hydrothermal synthesis of α-SnWO4: Application to lithium-ion battery and photocatalytic activity

The high capacity anode material is required to replace the most commonly used anode - graphite to keep up the global demand to achieve the goal. Multi-metal oxide has gained keen attention for its higher theoretical capacity and relatively stable than a single metal oxide. α-SnWO₄ has a theoretical capacity of 850 mAh g^?1 which is greater than graphite (372 mAh g^?1). α-SnWO₄ has been synthesized through low-temperature hydrothermal method using tin chloride and sodium tungstate as a precursor in acidic medium (succinic acid) at 200 °C for 12 h. The obtained product has been characterized using various analytical tools such as XRD, FT-IR, UV-DRS, BET, PL, SEM, and HR-TEM. XRD analysis shows the orthorhombic phase with a crystallite size of ~25 nm α-SnWO₄has been examined as an electrode material for Li-ion battery (LIB) and displays an initial discharge capacity of 985 mAh g^?1. Columbic efficiency close to 100% has been observed for 100 cycles. The stability of the electrode material was studied at different C-rates. Band-gap calculated using UV-DRS (Eg = 1.9 eV) shows that α-SnWO₄ is a good candidate for photocatalytic degradation. Results of the photocatalytic experiment using methylene blue (MB) as a model pollutant in an aqueous medium shows good results. The above applications show that α-SnWO₄ is multifunctional materials for diverse applications.