Preparation of Mn2SnO4 nanoparticles as the anode material for lithium secondary battery

The ultrafine Mn₂SnO₄ nanoparticles with diameters of 5-10 nm have been prepared by thermal decomposition of precursor MnSn(OH)₆. The MnSn(OH)₆ nanoparticles precursor was synthesized by a hydrothermal microemulsion method. X-ray diffraction, transmission electron microscopy, high-resolution transmission electron microscopy and electron diffraction have been employed to characterize the crystal structures and morphologies of the as-prepared samples. High-resolution transmission electron microscopy observations revealed that the as-synthesized nanoparticles were single crystals. The thermal characterization was studied by differential thermal analysis and thermogravimetry analysis measurements. Electrochemical test showed that the Mn₂SnO₄ nanoparticles exhibited a high initial charge-discharge capacity of 1320 mAh/g.     

Na2EDTA-assisted hydrothermal synthesis and luminescent properties of YVO4:Eu3+ with different morphologies in a wide pH range

Nano- and micro-scaled Eu-doped yttrium orthovanadate (YVO₄:Eu³⁺) powders had been fabricated via disodium ethylenediamine tetraacetate (Na₂EDTA)-assisted morphology controllable hydrothermal method in a wide pH range at 180 °C for 24 h. The as-synthesized samples were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and photoluminescence spectroscopy (PL). The results showed that the pH value of the synthesis solution played a key role in the formation of the final products with different morphologies, including ball-like micro-spheres, micro-spheres composed of submicron cubes and flower-like structures containing nano-plates. The photoluminescence measurement revealed that the luminescent properties of the samples were changed by varying their morphologies. The significant ball-like micro-spheres of YVO₄:Eu³⁺ particles had been synthesized, and the luminescence intensity of them is the strongest one among all products.     

Nonionic surfactant-assisted hydrothermal synthesis of YVO4:Eu3+ powders in a wide pH range and their luminescent properties

YVO₄:Eu³⁺ powders with different morphologies were fabricated by a simple hydrothermal method at 180 °C for 24 h in a wide pH range with the assistance of polyvinylpyrrolidone (PVP) as a nonionic surfactant. The as-synthesized samples were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and photoluminescence spectroscopy (PL). The obtained results showed that the pH value of synthesis solution played a key role in the formation of final products with different morphologies, such as, microspheres, irregular microspheres with grain-like nanoparticles, stone-like structures with regular short nanorods, and smooth rhombohedrons. The PL measurements revealed that the emission intensity of the samples was first decreased, and then increased with increasing the pH value due mainly to the increase in crystallinity and decrease in surface defects.     

Impact of reaction temperature,stirring and cosolvent on the solvothermal synthesis of anatase TiO2 and TiO2/titanate hybrid nanostructures: Elucidating the growth mechanism

One-dimensional anatase TiO₂ and hybrid TiO₂/titanate nanostructures are synthesized by a simple low temperature solvothermal route followed by the Na⁺/H⁺ ion-exchange and final calcination process. We investigated the impact of reaction temperature, stirring conditions and cosolvent on the morphologies of the as-prepared nanostructures. Nanotubes and nanorods are formed in alkaline solution, while nanorods/nanowires and nanoporous nanoribbons are formed in alkaline water–ethanol and alkaline water–ethylene glycol mixed solvents, respectively. X-ray diffraction, Raman scattering and high-resolution transmission electron microscopy studies are employed to identify the structure and phase composition. The formation of different morphologies of the as-synthesized nanostructures is investigated by field emission scanning electron microscopy and transmission electron microscopy. The growth mechanism and reaction process of the as-prepared nanostructures are explained based on the experimental observations. The photoluminescence, optical absorption and the tuning of band gap of the prepared samples are also studied. This work will be valuable for understanding the growth mechanism of various nanostructured TiO₂ and to explore the commercial applications of nanoporous nanoribbons of TiO₂.     

Controllable synthesis of hierarchical nanostructures of CaWO4 and SrWO4 via a facile low-temperature route

CaWO₄ and SrWO₄ nanostructures have been synthesized via a simple microemulsion-mediated route. With careful control of the fundamental experimental parameters including the concentration of reactants, the reaction time and the temperature, the products with different morphologies of dumbbell, coral, rod and dendrite have been obtained, respectively. The possible formation mechanism of these unique morphologies has been proposed based on surfactant self-assembly under different experimental conditions. The as-synthesized CaWO₄ samples with various morphologies exhibit different photoluminescence properties. X-ray powder diffraction, transmission electron microscopy, field-emission scanning electron microscopy, and luminescence spectroscopy were used to characterize these products.     

Controllable synthesis and luminescence properties of TiO2:Eu3+ nanorods,nanoparticles and submicrospheres by hydrothermal method

Eu³⁺-doped TiO₂ nanocrystals with three kinds of morphologies (nanorods, nanoparticles, and submicrospheres) have been successfully fabricated in cetyltrimethylammonium bromide (CTAB)/water/cyclohexane/n-pentanol reverse micelle by hydrothermal method for the first time and their photoluminescence (PL) properties have also been studied. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive spectroscopy (EDS), FT-IR, and PL spectra were used to characterize the samples. The acidic and alkaline conditions of the microemulsion play an important role in determining the geometric morphologies of the final products. TiO₂:Eu³⁺ with three different morphologies all exist only in anatase phase and show high luminescence intensity without further calcinations, which show its advantages of energy saving. The shape of emission spectra was independent of the morphologies of the products but the luminescence intensity of the TiO₂:Eu³⁺ materials is strongly dependent on their morphology. The results show that TiO₂:Eu³⁺ nanorods possess the strongest luminescence intensity among the three nanostructured samples.     

Sonochemical synthesis of luminescent CeCO3OH one-dimensional quadrangular prisms

Orthorhombic single-crystalline cerium carbonate hydroxide (CeCO₃OH) with one-dimensional (1D) microstructures has been successfully synthesized by a facile sonochemical reaction between cerous nitrate and urea. These 1D microstructures were characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM), field-emission scanning electron microscopy (FE-SEM). The as-synthesized CeCO₃OH has uniform lengths and good dispersion. Synthetic parameters, such as the concentration of reagents, were found to have close relationship with the morphologies and sizes of the final products. The ultrasound-induced oriented attachment growth mechanism has been proposed for the possible formation mechanism of sample. Room-temperature photoluminescence of CeCO₃OH samples with different morphologies has also been investigated.     

Synthesis RMn2O5 (R = Gd and Sm) nano- and microstructures by a simple hydrothermal method

Single-phase RMn₂O₅ (R = Gd and Sm) nano- and microstructures have been successfully synthesized via a simple hydrothermal process at 250 °C for 24 h using NaOH as mineralizer. X-ray diffraction (XRD), scanning electron microscopy (SEM), X-ray energy dispersive spectroscopy (EDS), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM) and selective area electron diffraction patterns (SAED) were used to characterize the as-synthesized GdMn₂O₅ and SmMn₂O₅ samples. The effect of NaOH concentration and the molar ratio of Mn²⁺/Mn⁷⁺ on the morphology and size of the final products was studied, and a possible formation mechanism of RMn₂O₅ (R = Gd and Sm) nanoplates and nanorods under hydrothermal conditions was proposed.     

Synthesis,characterization and catalytic property of manganese dioxide with different structures

In this paper, different crystallographic types and crystal morphologies of MnO₂ nanomaterials have been selectively synthesized by a simple hydrothermal route. α-MnO₂ nanowires, and γ-MnO₂ hollow hierarchical spheres have been prepared by a sodium dodecyl benzenesulfonate (SDBS)-assisted hydrothermal treatment method. The as-synthesized samples were characterized by XRD, SEM, TEM, and HRTEM. Furthermore, the obtained different kinds of MnO₂ nanostructures were found to exhibit favorable photocatalytic activity in organic dyestuff such as methyl orange, showing potential applications in photocatalysis. And the results showed that γ-MnO₂ hollow micro-spheres exhibited superior photocatalytic activities to α-MnO₂.     

Hydrothermal synthesis,characterization and luminescent properties of GdPO4·H2O:Tb nanorods and nanobundles

In this paper, the Tb³⁺-doped GdPO₄·H₂O nanorods and nanobundles have been synthesized by the hydrothermal method with and without glycine, respectively. The X-ray powder diffraction (XRD), thermogravimetric and differential thermal analysis (TG–DTA), Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), energy-dispersive spectra (EDS) and photoluminescence (PL) were employed to characterize the as-obtained products. It was found that the addition of glycine and the pH value have crucial influences on the formation of the resulting morphologies and sizes. The possible formation mechanisms for GdPO₄·H₂O:Tb³⁺ nanorods and nanobundles were put forward. A detailed investigation on the photoluminescence of GdPO₄·H₂O:Tb³⁺ different samples revealed that the luminescent properties of products are strongly correlated with the morphologies, sizes, coordination environment and crystal field symmetry.     

Synthesis of Cu11(OH)14(CrO4)4 nanobelts

Cu₁₁(OH)₁₄(CrO₄)₄ nanobelts have been synthesized by hydrothermal method in the absence of any surfactants. The as-synthesized products are characterized by X-ray diffraction, transmission electron microscopy, and scanning electron microscopy. The average thickness, widths and lengths of the nanobelts are about 15 nm, 40 nm, and several micrometers, respectively. It is interesting that Cu₁₁(OH)₁₄(CrO₄)₄ nanobelts are very sensitive to electron beam illumination. The influences of the reaction temperature on the morphologies of the resulting products have been investigated.     

Phase selection controlled by sodium ions in the synthesis of FAU/LTA composite zeolite

Abstract

Zeolite faujasite (FAU), Linde type A (LTA) and FAU/LTA composite have been synthesized using tetramethylammonium cation (TMA⁺) as template, by adjusting only the concentration of Na⁺ ions in the initial solution (1.00 Al₂O₃ 4.36 SiO₂ : 2.39 (TMA)₂ O : β Na₂ O : 249.00H₂ O). Na⁺ ions alter the phase composition of the product more than TMA⁺ or OH^? ions. When Na₂ O concentration [Na₂ O] increases from 0.024 to 0.168, the product gradually changes from pure FAU to pure LTA via the formation of FAU/LTA composite with increasing LTA fraction. Interestingly, the induction periods of FAU and LTA in the FAU/LTA composite zeolite ([Na₂ O] is 0.072) are both 13 h, quite different from the induction periods of their individual pure phases—45 h for FAU and 4 h for LTA. During the crystallization, the LTA/(FAU + LTA) fraction in the composite zeolite decreases in a nearly linear fashion. Scanning electron microscopy, thermogravimetry and differential thermal analysis indicate some difference between the properties of the FAU/LTA composite zeolite and of the mechanical mixture.     

A simple solvothermal reduction route to copper and cuprous oxide

Pure copper nanocrystallites and cuprous oxide nanorods have been synthesized via solvothermal treatment of CuSO₄ or CuSO₄·5H₂O and NaOH in pure ethanol and mixed solution of ethanol and deionized water at 140 °C for 10 h, respectively. Transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HRTEM) were used to investigate the different morphologies of the as-synthesized products. X-ray powder diffraction (XRD) and selected area electron diffraction (SAED) were applied to characterize the composition and crystal phases of the products. It was proposed that the reducibility of ethanol was influenced by temperature and the addition of deionized water in the formation of different phases, which were realized by carefully controlling the experimental conditions.     

Controlled synthesis of different morphological YF3 crystalline particles at room temperature

YF₃ crystalline particles with different crystal structures and different morphologies have been synthesized via a simple solution route by varying the fluoride source (NH₄F, HF, NH₄F·HF) and molar ratio of Y³⁺/F⁻ at room temperature. They were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) and X-ray photoelectron spectrum (XPS).     

Synthesis of (K, Na)NbO3 particles by high temperature mixing method under hydrothermal conditions

In order to prepare the pure (K, Na)NbO₃(KNN) particles with higher crystallinity, the high temperature mixing method (HTMM) under hydrothermal conditions was carried out in this work. The obtained samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED), and high-resolution transmission electron microscopy (HRTEM). The results indicate that the KNN particles size decrease gradually with the increase of mineralization concentration in the starting solution. The ratio of K⁺/(K⁺ + Na⁺) in the starting solution has a great effect on the phase of the products, and several phases coexist in the product when the ratio of K⁺/(K⁺ + Na⁺) in the starting solution is 0.7.     

Synthesis and characterization of porous sphere-like ZnO with dendrite nanocrystals from layered inorganic-organic nanocomposite on titanium substrate

The porous sphere-like ZnO inorganic-organic nanocomposites have been prepared by self-assembly at the present of CTAB (cetyltrimethylammonium bromide, CH₃(CH₂)₁₅N⁺(CH₃)₃Br⁻) surfactant on the titanium substrate. After high temperature oxidation, all the organic were removed and the porous sphere-like ZnO dendrite nanocrystals were obtained. The resultant products have been characterized by X-ray powder diffraction (XRD), field emission scanning electron microscopy (FE-SEM), and transmission electron microscopy (TEM). The XRD pattern shows that the as-synthesized porous sphere-like is multilayered inorganic-organic nanocomposite, and the sample calcined at 500 °C for 2 h has a hexagonal wurtzite crystal structure. FE-SEM and TEM images demonstrate that porous sphere-like ZnO dendrite nanocrystals are formed. A possible formation mechanism is preliminary proposed for the formation of the novel nanostructure.     

Sol–gel assisted hydrothermal synthesis of ZnO microstructures: Morphology control and photocatalytic activity

ZnO microstructures of different morphologies were synthesized by the sol–gel assisted hydrothermal method using Zn(NO₃)₂, citric acid and NaOH as raw materials. Twining-hexagonal prism, twining-hexagonal disk, sphere and flower-like ZnO microstructures could be synthesized only through controlling the pH of the hydrothermal reaction mixture at 11, 12, 13 and 14, respectively. The as-synthesized samples were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM). Optical properties were examined by UV–Vis absorption/diffuse reflectance spectroscopy and room-temperature photoluminescence measurements (PL). Photocatalytic activities of the samples were evaluated by degradation of Reactive Blue 14 (KGL). The results indicated that the flower-like ZnO composed of nanosheets possessed superior photocatalytic activity to other ZnO microstructures and commercial ZnO, which could be attributed to the morphology, surface defects, band gap and surface area. The formation mechanisms of different ZnO morphologies were also investigated based on the experimental results.     

Influence of the Eu3+ dosage concentration on luminescence properties of YPO4:Eu3+ microspheres

In this study, YPO₄:Eu³⁺ microspheres with different Eu³⁺ dosage concentration were fabricated by a facile hydrothermal route at 200 °C for 10 h in the presence of citric acid. The YPO₄:Eu³⁺ samples were characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), and luminescence spectroscopy. The XRD results reveal that the YPO₄:Eu³⁺ samples presented a tetragonal structure. The TEM and SEM observations demonstrate that the YPO₄:Eu³⁺ samples with uniform sphere-like morphologies can be obtained at 200 °C for 10 h. The sizes of samples are in the range of 2–2.2 μm. The room temperature luminescence properties of YPO₄:Eu³⁺ samples were studied using an excitation wavelength of 227 nm. The emission spectrum displays the bands associated to the ⁵D₀ → ⁷F_J (J = 1, 2 and 4) electronic transitions characteristics of the Eu³⁺ cations at different positions. The influence of Eu³⁺ dosage concentration on luminescence properties of YPO₄:Eu³⁺ microspheres were studied carefully.     

D-penicillamine assisted hydrothermal synthesis of Bi2S3 nanoflowers and their electrochemical application

Single crystalline flower-like Bi₂S₃ nanostructures were successfully synthesized via a simple, facile and green hydrothermal method, with the assistance of D-penicillamine. The products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM), and found their morphologies mainly depend on the ratios of Bi^3 + to D-penicillamine, as well as the reaction temperature and time. And the possible growth mechanism has been discussed in some detail. In addition, the as-prepared Bi₂S₃ nanoflowers show good hydrogen storage ability. This strategy can be potentially expanded to prepare other metal chalcogenides materials.     

Ionothermal synthesis of AlPO4 molecular sieves in the presence of quaternary ammonium cation

Several aluminophosphate molecular sieves were synthesized ionothermally, in ionic liquid 1-butyl-3-methyl imidazolium bromide ([BMIm]Br) with adding various quaternary ammonium cation (quats, including tetramethyl ammonium (TMA⁺), choline, tetraethyl ammonium (TEA⁺), tetrapropyl ammonium (TPA⁺) and tetrabutyl ammonium (TBA⁺)). These products were characterized by X-ray diffraction (XRD), ¹³C nuclear magnetic resonance (NMR) and scanning electron microscope (SEM). The result indicates that the crystallization pathway is changed by adding these quats. AlPO₄-42 (IZA code LTA) crystallizes when TMA⁺ is added in the system, AlPO₄-5 (AFI) crystallizes when choline or TEA⁺ is added, and the AlPO₄-11 (AEL) crystallizes when TPA⁺ or TBA⁺ is added. ¹³C NMR analysis indicates that these introduced quats may either replace the [BMIm]⁺ to act as template alone, or direct structures cooperatively with the [BMIm]⁺, or in some cases they cannot change the original structure directing effect of [BMIm]⁺.