Synthesis and characterisation of SnO2 nano-single crystals as anode materials for lithium-ion batteries

Rutile structure SnO₂ nano-single crystals have been synthesized using tin (IV) chloride as precursor by the modified hydrothermal method. Controllable morphology and size of SnO₂ could be obtained by adjusting the concentration of the hydrochloric acid. The SnO₂ nanoparticles were characterised by transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), scanning electron microscopy (SEM), X-ray diffraction (XRD) and electrochemical methods. The SnO₂ nanoparticles as anode materials in lithium-ion batteries exhibit high lithium storage capacities. The reversible capacities are more than 630 mA h g^− 1.     

Synthesis of single-crystalline Ce(CO3)(OH) with novel dendrite morphology and their thermal conversion to CeO2

Single-crystalline cerium carbonate hydroxide (Ce(CO₃)(OH)) with dendrite morphologies have been successfully synthesized by hydrothermal method at 150 °C using Ce(NO₃)₃·6H₂O as the cerium source, aqueous carbamide as both an alkaline and carbon source and poly(vinyl pyrrolidone) (PVP) as surfactant. Ceria (CeO₂) with dendrite morphologies have been fabricated by a thermal decomposition-oxidation process at 500 °C for 6 h using single-crystalline Ce(CO₃)(OH) dendrites as the precursor. The dendrite morphologies of Ce(CO₃)(OH) was sustained after thermal decomposition-oxidation to CeO₂. The as-prepared products were characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM), field-emission scanning electron microscopy (FE-SEM), and thermogravimetric analysis (TG).     

CuSn(OH)6 submicrospheres: Room-temperature synthesis, growth mechanism, and weak antiferromagnetic behavior

CuSn(OH)₆ submicrospheres with diameters of 400-900 nm have been successfully fabricated using a simple aqueous solution method at room temperature. Influencing factors such as the dosage of reactants and reaction time on the preparation were systematically investigated. The products were characterized with X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), thermogravimetric analysis (TG) and differential thermal analysis (DTA). Results reveal that the CuSn(OH)₆ spheres are built from numerous nanoparticles. It is found that the diameter of CuSn(OH)₆ spheres can be readily tuned by adjusting the molar ratio of to Cu²⁺. A possible growth mechanism for the CuSn(OH)₆ submicrospheres has been proposed. Amorphous CuSnO₃ submicrospheres were obtained after thermal treatment of the CuSn(OH)₆ submicrospheres at 300 °C for 4 h. Standard magnetization measurements demonstrate that the CuSn(OH)₆ submicrospheres are antiferromagnetic and have a weak spin-Peierls transition at about 78 K.     

Controlled synthesis of Mn3O4 and MnCO3 in a solvothermal system

Controlled synthesis of Mn₃O₄ nanocrystals and MnCO₃ aggregates was achieved by a facile solvothermal method using different divalent manganese source in the solvent of N,N-dimethylformamide (DMF) with/without the introduction of poly(vinylpyrrolidone) (PVP). PVP was used as a co-reducing reagent in the controlled formation of MnCO₃ crystal. The products were characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM) and selected-area electron diffraction (SAED), Fourier transform infrared (FTIR) spectra, Raman spectrum and magnetic measurement. Higher process temperature and longer solvothermal time were favorable for the formation of MnCO₃ single phase using MnCl₂ as the manganese source. Mn₃O₄ nanocrystals were prepared at a relatively lower temperature. MnCO₃ aggregates consisted by small nanoparticles have a certain orientation, showing that the nanocrystals formed earlier through oriented aggregation. The size of Mn₃O₄ nanocrystals was 22.5 ± 7.3 nm and 7.3 ± 1.4 nm prepared using MnCl₂ and Mn(CH₃COO)₂, respectively, at 160 °C for 24 h. Raman spectra showed size-dependent characteristics. Smaller Mn₃O₄ nanoparticle resulted in a red-shift in Raman spectra. Magnetic property of the prepared Mn₃O₄ nanoparticle was influenced by the size distribution and crystallinity.     

Synthesis and spectroscopic investigations of Mn3O4 nanoparticles

Trimanganese tetraoxide (Mn₃O₄) nanoparticles have been synthesized via hydrothermal process. Nevertheless, homogeneous nanoparticles of Mn₃O₄ with platelet lozange shape were obtained. The crystallite size ranged from 40 to 70 nm. The Mn₃O₄ product was investigated by X-ray diffraction, transmission electron microscopy (MET), and impedance spectroscopy. Electrical conductivity measurements showed that the as-synthesized Mn₃O₄ nanomaterial has a conductivity value which goes from 1.8 10⁻⁷ Ω⁻¹ cm⁻¹ at 298 K, to 23 10⁻⁵ Ω⁻¹ cm⁻¹ at 493 K. The temperature dependence of the conductivity between 298 and 493 K obeys to Arrhenius law with an activation energy of 0.48 eV.     

Solution synthesis and electrochemical capacitance performance of Mn3O4 polyhedral nanocrystals via thermolysis of a hydrogen-bonded polymer

Hausmannite Mn₃O₄ polyhedral nanocrystals have been successfully synthesized via a simple solution-based thermolysis route using a three-dimensional hydrogen-bonded polymer as precursor. The as-obtained product was characterized by means of powder X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM). Possible formation mechanism of polyhedral nanocrystals was proposed based on the role of organic ligand dissociation from the polymer precursor at elevated temperature. The electrochemical capacitance performance of Mn₃O₄ electrode was investigated by cyclic voltammetry and galvanostatic charge/discharge measurements. A maximum specific capacitance of 178 F g⁻¹ was obtained for the nanocrystals in a potential range from −0.1 to 0.8 V vs. SCE in a 0.5 M sodium sulfate solution at a current density of 0.2 A g⁻¹.     

Low temperature synthesis of nanocrystalline Li4Mn5O12 by a hydrothermal method

A mild hydrothermal method using Li-birnessite (Li_xMnO₂·nH₂O) ultrafine fiber as the precursor has been adopted to prepare Li₄Mn₅O₁₂, which is of interest as an electrode material for 3 V rechargeable lithium ion batteries. X-ray diffraction data reveal that the obtained powders have a pure spinel structure with a lattice constant of 8.135 Å. The scanning electron microscopy image of the obtained powders shows the particles are cubic-shaped whose average size is about 40-50 nm. The results from inductively coupled plasma-atomic emission spectroscope and wet chemical analysis indicate that a Li/Mn ratio of 0.796, and an average valence of 3.96 of Mn ion have been achieved in the as-prepared products. The thermogravimetric and differential thermal analysis data also agree with the previous reports on Li₄Mn₅O₁₂, suggesting that near stoichiometry of Li₄Mn₅O₁₂ has been synthesized by this procedure at the rather low temperature 110°C.     

Preparation and luminescence properties of Mn-doped ZnGa2O4 nanofibers via electrospinning process

One-dimensional Mn²⁺-doped ZnGa₂O₄ nanofibers were prepared by a simple and cost-effective electrospinning process. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), thermogravimetric and differential thermal analysis (TG-DTA), scanning electron microscopy (SEM), energy-dispersive X-ray spectrum (EDS), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), photoluminescence (PL) and cathodoluminescence (CL) spectra as well as kinetic decays were used to characterize the samples. SEM results indicated that the as-formed precursor fibers and those annealed at 700 °C are uniform with length of several tens to hundred micrometers, and the diameters of the fibers decrease greatly after being heated at 700 °C. Under ultraviolet excitation (246 nm) and low-voltage electron beams (1–3 kV) excitation, the ZnGa₂O₄:Mn²⁺ nanofibers presents the blue emission band of the ZnGa₂O₄ host lattice and the strong green emission with a peak at 505 nm corresponding to the ⁴T₁–⁶A₁ transition of Mn²⁺ ion.     

Synthesis and characterization of NiFe2O4 nanosheet via polymer assisted co-precipitation method

Nickel ferrite (NiFe₂O₄) nanosheet has been synthesised by the polymer assisted co-precipitation method. The synthesised nanosheet was characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), high-resolution scanning electron microscopy (HRSEM), thermal analysis and vibrating sample magnetometry (VSM). The results showed that the as synthesised NiFe₂O₄ has sheet like morphology with good crystalline nature. The nanosheet was formed through random aggregation of magnetic nanoparticles. Ferromagnetic property was exhibited by the nanosheet with saturation magnetization M_s = 35 emu/g, remanent M_r = 8.6 Oe and coercive force H_c = 192 emu/g.     

Microwave-assisted synthesis of cobalt oxalate nanorods and their thermal conversion to Co3O4 rods

Cobalt oxalate nanorods have been successfully synthesized by a simple microwave-assisted solution approach using an ionic liquid 1-n-butyl-3-methyl imidazolium tetrafluoroborate. Upon thermal decomposition at 400 °C, cobalt oxalate nanorods could be converted to Co₃O₄ rods consisting of nanoparticles. The products were characterized using X-ray powder diffraction, transmission electron microscopy, thermogravimetric analysis and differential scanning calorimetric analysis.     

Photocatalytic hydrogen production over Na2Ti2O4(OH)2 nanotube sensitized by CdS nanoparticles

Na₂Ti₂O₄(OH)₂ nanotubes were obtained by hydrothermal reaction of TiO₂ with concentrated NaOH solution. CdS nanoparticles were then decorated on Na₂Ti₂O₄(OH)₂ nanotubes through partial ion-exchange method. The composite photocatalysts were characterized by X-ray diffraction (XRD), ultraviolet-visible spectra (UV-vis), transmission electron microscope (TEM), etc. The results showed that CdS nanoparticles of 5-6 nm were anchored on the surface of the Na₂Ti₂O₄(OH)₂ nanotubes. Under irradiation of visible light (λ ≥ 430 nm), the prepared CdS/Na₂Ti₂O₄(OH)₂ showed high photoactivity for hydrogen production.     

Sub-2 nm SnO2 nanocrystals: A reduction/oxidation chemical reaction synthesis and optical properties

A simple reduction/oxidation chemical solution approach at room temperature has been developed to synthesize ultrafine SnO₂ nanocrystals, in which NaBH₄ is used as a reducing agent instead of mineralizers such as sodium hydroxide, ammonia, and alcohol. The morphology, structure, and optical property of the ultrafine SnO₂ nanocrystals have been characterized by high-resolution transmission electron microscopy (HRTEM), X-ray powder diffraction (XRD), differential scanning calorimetry and thermogravimetric analysis (DSC-TGA), X-ray photoelectron spectroscopy (XPS) and UV-vis absorption spectroscopy. It is indicated that the uniform tetragonal ultrafine SnO₂ nanocrystals with the size below 2 nm have been fabricated at room temperature. The band gap of the ultrafine SnO₂ nanocrystals is about 4.1 eV, exhibiting 0.5 eV blue shift from that of the bulk SnO₂ (3.6 eV). Furthermore, the mechanism for the reduction/oxidation chemical reaction synthesis of the ultrafine SnO₂ nanocrystals has been preliminary presented.     

CuSn(OH)6 submicrospheres: Room-temperature synthesis and weak antiferromagnetic behavior

CuSn(OH)₆ submicrospheres with a diameter of 400-900 nm, which are composed of nanoparticles with a size of about 27.8 nm, have been successfully synthesized for the first time via a simple liquid approach at room temperature in 15 min. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) were used to characterize the products. Standard magnetization measurements at low temperature reveal that the as-obtained CuSn(OH)₆ submicrospheres are antiferromagnetic and have a weak spin-Peierls transition at about 78 K.     

Synthesis and characterization of nanocrystalline MgAl2O4 spinel via sucrose process

Nanocrystalline MgAl₂O₄ spinel powder was synthesized using metal nitrates and a polymer matrix precursor composed of sucrose and polyvinyl alcohol (PVA). The precursor and the calcined powders were characterized by simultaneous thermal analysis (STA), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). According to XRD results, the inceptive formation temperature of spinel via this technique was between 600 and 700 °C. The calcined powder at 800 °C for 2 h has faced shaped morphology and its crystallite size is in the range of 8-12 nm. Further studies also showed that the amount of polymeric matrix to metal ions has significant influence on the crystallite size of synthesized magnesium aluminate spinel powder.     

CuS nanotubes prepared using Cu(OH)2 nanowires as self-sacrificial template

Copper sulfide (CuS) nanotubes assembled with nanoparticles have been successfully synthesized by microwave-assisted solvothermal method at 80 °C using Cu(OH)₂ nanowires in the solvent of ethylene glycol. Cu(OH)₂ nanowires act as both the precursor and template for the preparation of CuS nanotubes assembled with nanoparticles. Cu(OH)₂ nanowires are prepared by adding an aqueous solution containing CuCl₂ into an alkaline solution at room temperature and by ultrasonication for 30 min. This method has the advantages of the simplicity and low cost. The samples are characterized by X-ray powder diffraction (XRD) and transmission electron microscopy (TEM). The method reported herein may be extended to the synthesis of nanotubes of other copper-containing compounds.     

Green hydrothermal synthesis and characterization of CdO2 nanoparticles

A green hydrothermal method has been developed for the synthesis of CdO₂ nanoparticles from Cd(OH)₂ powder and 6 vol.% H₂O₂ aqueous solution at 80-150 °C. The characterization results from X-ray diffraction, transmission electron microscopy, and thermal gravimetric and differential scanning calorimetry analysis disclosed that the resultant products were pure cubic phase CdO₂ nanoparticles with the sizes in the range of about 11-13 nm. The UV-vis absorption spectra revealed that the as-synthesized CdO₂ nanoparticles had similar optical band gaps of about 3.85 eV. The Raman spectra of the as-synthesized CdO₂ nanoparticles displayed two obvious peaks at about 348 and 830/833 cm^-1, a characteristic of pyrite-type IIB-peroxides.     

Size and morphology-controlled Ni2[Fe(CN)6]·xH2O Prussian Blue analogue fabricated via a hydrothermal route

Nanocrystalline Prussian Blue analogue Ni₂[Fe(CN)₆]·xH₂O was synthesized through hydrothermal process at 180 °C for 24 h with NiSO₄·6H₂O and K₄[Fe(CN)₆]·3H₂O as precursors. The effects of reactant concentration and protective matrix (Polyethylene glycol 400, PEG-400) on the size and morphology of nanoparticles were investigated. The as-synthesized products were identified as face-centered cubic structure by powder X-ray diffraction. Field-emission scanning electron microscopy and transmission electron microscopy images showed that well dispersed nanoparticles with fairly narrow size distribution were successfully prepared.     

Synthesis of stable spherical platinum diphosphide, PtP2/carbon nanocomposite by reacting Pt(PPh3)4 at elevated temperature under autogenic pressure

The synthesis of microsized carbon spheres supporting the semiconductor platinum diphosphide, PtP₂, was conducted by the thermal decomposition of an organometallic precursor. This novel reaction was carried out using the reaction under autogenic pressure at elevated temperature (RAPET) method by dissociating Pt(PPh₃)₄ at 1000 °C. The product was characterized using methods of electron microscopy (scanning electron microscope (SEM), transmission electron microscope (TEM), selected area energy dispersive spectroscopy (SAEDS), elemental analyzer (EA) and energy dispersive X-ray analysis (EDX)) and powder-XRD. Transmission electron microscope images indicate that the particle size of the nanoparticles of PtP₂ coated on the carbon spheres is 50 nm.     

Synthesis, morphology and optical properties of multi-pods Au/FeO(OH) and Au/Fe2O3 nanostructures

Multi-pods Au/FeOOH nanostructures were synthesized by a hydrothermal treatment of an aqueous solution of mixed micellar formed by gold nanoparticles, hexadecyltrimethyl ammonium bromide (CTAB), and (NH₄)₃[FeF₆] at 160 °C for 48 h and sequential calcined at 290 °C for 1.5 h, resulting in the formation of multi-pods Au/Fe₂O₃ nanostructures. The as-obtained products were characterized by powder X-ray diffraction, transmission electron microscopy, selected area electron diffraction, field emission scanning electron microscopy, and UV-vis spectroscopy. Surface plasmon resonance band of gold nanoparticles was observed in the multi-pods Au/FeOOH nanostructures. However, a similar behavior was not seen with multi-pods Au/Fe₂O₃ nanostructures. The critical role of F⁻ ions and CTAB molecules in the formation of FeO(OH) multipods and the probable mechanism of the formation of multi-pods Au/FeOOH and Au/Fe₂O₃ nanostructures were discussed.     

Thermal, dielectric and microwave absorption properties of polyaniline-CoFe2O4 nanocomposites

The present paper deals with the synthesis of conducting ferromagnetic polyaniline-CoFe₂O₄ (PC) nanocomposites via one-step chemical oxidative polymerization of aniline in the presence of CoFe₂O₄ nanoparticles (30-40 nm). These nanocomposites of PC have been characterized by high-resolution transmission electron microscopy (HRTEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA) and vibrating sample magnetometer (VSM). Extended thermal analysis has revealed that the activation energy of these nanocomposites varies from 75.3 to 84.3 kJ/mol as compared to the activation energy of 50.3 kJ/mol for polyaniline-DBSA. In addition, dielectric and microwave absorption properties of the nanocomposites have been measured in the frequency range of 12.4-18 GHz (Ku-band) which demonstrate that more than 99% attenuation of microwaves (SE_A = 21.5 dB) has been achieved using these nanocomposites. Systematic investigations reveal that the CoFe₂O₄ nanoparticles in the polyaniline matrix have phenomenal effect in determining the microwave absorption properties of the nanocomposites.