Characterization of nanosized Al2(WO4)3

Nanosized aluminum tungstate Al₂(WO₄)₃ was prepared by co-precipitation reaction between Na₂WO₄ and Al(NO₃)₃ aqueous solutions. The powder size and shape, as well as size distribution are estimated after different conditions of powder preparation. The purity of the final product was investigated by XRD and DTA analyses, using the single crystal powder as reference. Between the specimen and the reference no difference was detected. The crystal structure of Al₂(WO₄)₃ nanosized powder was confirmed by TEM (SAED, HRTEM). In additional, TEM locality allows to detect some W₅O₁₄ impurities, which are not visible by conventional X-ray powder diffraction and thermal analyses.     

Solvothermal synthesis of fusiform hexagonal prism SrCO3 microrods via ethylene glycol solution

Fusiform hexagonal prism SrCO₃ microrods were prepared by a simple solvothermal route at 120 °C, and characterized by X-ray powder diffraction (XRD), field-emission scanning electron microscopy (FE-SEM) and Fourier transform infrared (FT-IR) spectroscopy. By controlling the content of ethylene glycol (EG), it was found that ethylene glycol (EG) played an important role in the formation of such SrCO₃ microrods. Finally, effects of other solvents on the products, including 1,2-propanediol and glycerin, were also investigated.     

Hydrothermal synthesis and magnetic properties of Co0.2Cu0.03Fe2.77O4 nanoparticles

Co_0.2Cu_0.03Fe_2.77O₄ nanoparticles with different morphologies have been synthesized directly via a simple hydrothermal method. The effects of pH value, precursor concentration, reaction temperature and surfactant on the particle size were discussed. X-ray diffraction analyses showed that the as-synthesized Co_0.2Cu_0.03Fe_2.77O₄ nanoparticles possessed typical spinel structure. Scanning electron microscope images showed different morphologies of the particles, including truncated octahedron and octahedron. It was indicated that well-dispersed Co_0.2Cu_0.03Fe_2.77O₄ nanoparticles can be synthesized at pH values ranging from 11 to 13, and reaction temperature of 160 °C. The particle size decreased from 18 to 10 nm after the addition of sodium dodecyl sulphate at the pH value of 9. The magnetic measurement showed that the as-prepared Co-Cu spinel ferrite nanoparticles possessed hard magnetic property.     

Effect of KCl, NaCl and CaCl2 mixture on volume combustion synthesis of TiB2 nanoparticles

Preparation of titanium diboride (TiB₂) nanoparticles was carried out by volume combustion synthesis. TiO₂, B₂O₃ and elemental Mg were mixed with 0-60% salt mixture of KCl, NaCl and CaCl₂ with increment of 15% as a low melting temperature diluent. Compressed samples were synthesized in a tubular furnace at a constant heating rate under argon atmosphere. Thermal analysis of the process showed that the addition of the low melting temperature salts mixture led to a significant decrease in ignition and combustion temperatures. Synthesized samples were then leached by nitric and hydrochloric acids to remove impurities. The samples were examined by XRD, SEM and DLS analysis. The results showed the formation of fine deagglomerated particles with the addition of the salts mixture. The results revealed that 45% salts mixture had the smallest average particle size of about 90 nm.     

Powder synthesis and characterization of nanocrystalline CeO2 via the combustion processes

Nanocrystalline CeO₂ powders were synthesized by the combustion reactions using citric acid and glycol as fuels and nitrate as an oxidant. The adiabatic flame temperatures in the auto ignition processes of the precursors were calculated theoretically. XRD measurements indicated that the powders produced in the combustion processes were cubic fluorite CeO₂ phase. The size and morphology of the particles and extent of agglomeration in the powders were studied using transmission electron microscopy (TEM) and the particle size analyzer respectively. Blue shifts of the absorption peak of the as-prepared powders were observed.     

A new iron lead vanadate Pb2FeV3O11: Synthesis and some properties

A new iron lead vanadate, Pb₂FeV₃O₁₁, has been obtained. It melts incongruently at 650 ± 5 °C depositing two solid phases: Pb₂V₂O₇ and Fe₂O₃. Pb₂FeV₃O₁₁ crystallises in the monoclinic system. The infra-red spectrum and images of the new phase obtained by means of an electron scanning microscope are presented.     

Synthesis of hierarchical Ni11(HPO3)8(OH)6 superstructures based on nanorods through a soft hydrothermal route

In this paper, we reported the successful synthesis of hierarchical Ni₁₁(HPO₃)₈(OH)₆ superstructures based on nanorods via a facile hydrothermal route, employing NiCl₂·6H₂O and NaH₂PO₂·H₂O as the reactants in the presences of polyvinylpyrrolidone (PVP) and CH₃COONa·3H₂O. The reaction was carried out at 170 °C for 10 h. HPO₃²⁻ ions were provided via the dismutation reaction of H₂PO₂⁻ ions in a weak basic solution. The as-obtained products were characterized by X-ray powder diffraction (XRD), energy dispersive spectrometry (EDS), field emission scanning electron microscopy (SEM), selected area electron diffraction (SAED) and high resolution transmission electron microscopy (HRTEM). Some factors influencing the morphology of the hierarchical Ni₁₁(HPO₃)₈(OH)₆ nanorods, such as the reaction temperature, time, the amounts of PVP and CH₃COONa, and the initial concentration of Ni²⁺ ions, were systematically investigated. A possible growth mechanism was proposed based on experimental results.     

The system Ag2Se-Ho2Se3 in the 0-50 mol.% Ho2Se3 range and the crystal structure of two polymorphic forms of AgHoSe2

The phase diagram of the Ag₂Se-Ho₂Se₃ system in the range of 0-50 mol.% Ho₂Se₃ was constructed with the results of XRD and differential thermal analysis. A dimorphous compound exists in the system at the equimolar ratio of the components. The investigated part of the Ag₂Se-AgHoSe₂ diagram is of the eutectic type with the eutectic coordinates 7 mol.% Ho₂Se₃ and 1125 K. The crystal structure of the high-temperature modification of AgHoSe₂ was studied by X-ray powder diffraction method. α-AgHoSe₂ is described as a NaCl structure (space group ) with the lattice parameter а = 5.7623(3) Å. Atomic parameters were calculated in the isotropic approximation (R_I = 0.0434 and R_Р = 0.0636). The crystal structure of β-AgHoSe₂ was determined by X-ray structure analysis and was refined to R = 0.0487.     

The synthesis and selected properties of new compounds: Mg3Fe4(VO4)6 and Zn3Fe4(VO4)6

New compounds: Mg₃Fe₄(VO₄)₆ and Zn₃Fe₄(VO₄)₆ were obtained from a solid state reaction. The temperatures of melting of Mg₃Fe₄(VO₄)₆ and Zn₃Fe₄(VO₄)₆ amount to 950±5 and 850±5°C, respectively. The indexing results and the calculated unit cell parameters for both compounds are given and suggest that both phases are isotypic with Mn₃Fe₄(VO₄)₆. The IR spectra of the above-mentioned compounds are presented.     

Template-free synthesis of ZnWO4 powders via hydrothermal process in a wide pH range

ZnWO₄ powders with different morphologies were fabricated through a template-free hydrothermal method at 180 °C for 8 h in a wide pH range. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), UV-visible and luminescence spectrophotometers were applied to study the effects of pH values on crystallinity, morphology, optical and luminescence properties. The XRD results showed that the WO₃ + ZnWO₄, ZnWO₄, and ZnO phases could form after hydrothermal processing at 180 °C for 8 h with the pH values of 1, 3-11, and 13, respectively. The SEM and TEM observation revealed that the morphological transformation of ZnWO₄ powders occurred with an increase in pH values as follows: star anise-, peony-, and desert rose-like microstructures and soya bean- and rod-like nanostructures. The highest luminescence intensity was found to be in sample consisting of star anise-like crystallites among all the samples due to the presence of larger particles with high crystallinity resulted from the favorable pH under the current hydrothermal conditions.     

Synthesis and upconversion emission of rare earth-doped olive-like YF3 micro-particles

The olive-like YF₃ micro-particles were fabricated via a two-step route. The precursor NH₄Y₃F₁₀ nano-cages sized 8 nm with hollow interiors were first synthesized in a solid reaction at room temperature. In the course of subsequent hydrothermal treating, the unstable NH₄Y₃F₁₀ nano-cages were decomposed, resulted in the formation of Y(OH)_1.63F_1.37 micro-tubes. Prolonging the hydrothermal reaction induced the further decomposition of Y(OH)_1.63F_1.37 to produce YF₃ nano-crystals, which then aggregated together forming the final olive-like YF₃ micro-particles. For the Er³⁺/Yb³⁺ co-doped olive-like YF₃ micro-particles, intense visible upconversion emissions were measured under 976 nm excitation owing to the partition of rare earth ions in the lattice, indicating this material a promising luminescent host.     

A novel broadband emission phosphor Ca2KMg2V3O12 for white light emitting diodes

A novel broadband emission phosphor Ca₂KMg₂V₃O₁₂ was first synthesized by solution combustion method. The X-ray diffraction showed that Ca₂KMg₂V₃O₁₂ phase can be obtained at 600-900 °C through combustion route. The crystal structure of this material was refined by Rietveld method using powder X-ray diffraction. It crystallizes in cubic system and belongs to space group Ia3d with z = 8, a = 0.12500 nm. The excitation band of Ca₂KMg₂V₃O₁₂ peaks at 320 nm in a region between 260 nm and 425 nm, and the emission spectrum exhibits an intense band centered at about 528 nm covering from 400 nm to 800 nm. The colour coordinates of samples prepared at different ignition temperatures are in a range of x = 0.323-0.339, y = 0.430-0.447.     

Controllable synthesis and optical properties of NdOHCO3 dodecahedral microcrystals

NdOHCO₃ dodecahedral microcrystals with an orthorhombic structure have been successfully synthesized by the hydrothermal method used urea as the precipitator. Experimental parameters, such as the reaction temperature, the reaction time, and the molar ratio of the starting reagents were examined. The as-synthesized products were characterized by powder X-ray diffraction, transmission electron microscopy, field-emission scanning electron microscopy, X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy, and photoluminescence. The possible growth process of NdOHCO₃ dodecahedral microcrystals was discussed.     

Fabrication of microspherical LiMnPO4 cathode material by a facile one-step solvothermal process

The microspherical LiMnPO₄ cathode material was successfully prepared for the first time by a simple one-step solvothermal process in the presence of critic acid. The reaction conditions (reactant concentration, reaction temperature) were used further to fabricate the size, surface coarseness and morphology of the microspherical LiMnPO₄. The as-prepared microspherical LiMnPO₄ at variant conditions exhibited remarkably different discharge capacity and rate capacity, indicating the potential of the suggested method in tuning the morphology and the structure of LiMnPO₄ to improve its electrochemical performance.     

Structural study and luminescence of TlSrLa(AsO4)2

This work presents the crystal structure and luminescent properties of TlSrLa(AsO₄)₂. In this phase Tl⁺ ions are located in large tunnels delimited by chains of alternating (AsO₄) and (Sr,La)O₈ polyhedra. Thallium atoms are eightfold coordinated with C₁ symmetry. Large TlO distances are observed revealing a low stereochemical activity of the 6s² lone pair. Excitation and emission spectra of Tl⁺ in TlSrLa(AsO₄)₂ showed broad bands at lower energy than those observed in previous works. Excitation spectra are decomposed into multiple Gaussian bands and a theoretical analysis is made to explain the number of observed components. Two Gaussian components are revealed for emission spectra.     

Fabrication of porous TiO2 nanofiber and its photocatalytic activity

Porous TiO₂-based nanofiber was fabricated via a combined electrospinning and alkali-dissolution method. TiO₂/SiO₂ composite nanofiber was firstly prepared by electrospinning and sintering, and then silica was leached out with alkaline solution from the bulk of TiO₂/SiO₂ composite nanofiber to produce porous microstructure. The thermal decomposition and phase structure of the composite nanofiber precursor was investigated with TG/DSC and XRD, and optimal sintering temperature was obtained. SEM-EDX and FT-IR characterization show that most silica can be dissolved out from the composite nanofiber and thus porous nanofiber with excellent microstructure can be spontaneously formed. The effect of composite nanofiber composition on porous microstructure was studied, and it is found that the composite nanofiber with 20wt% silica can produce better porous microstructure compared to those with 10wt% and 30wt% silica. Meanwhile, porous TiO₂ nanofiber with 20wt% silica shows higher degradation efficiency to Congo Red.     

[NH3(CH2)2NH3][Co(SO4)2(H2O)4]: Chemical preparation, crystal structure, thermal decomposition and magnetic properties

Cobalt ethylenediammonium bis(sulfate) tetrahydrate, [NH₃(CH₂)₂NH₃][Co(SO₄)₂(H₂O)₄], has been synthesised by slow evaporation at room temperature. It crystallises in the triclinic system, space group , with the unit cell parameters: a = 6.8033(2), b = 7.0705(2), c = 7.2192(3) Å, α = 74.909(2)°, β = 72.291(2)°, γ = 79.167(2)°, Z = 1 and V = 317.16(2) Å³. The Co(II) atom is octahedrally coordinated by four water molecules and two sulfate tetrahedra leading to trimeric units [Co(SO₄)₂(H₂O)₄]. These units are linked to each other and to the ethylenediammonium cations through OW-H…O and N-H…O hydrogen bonds, respectively. The zero-dimensional structure is described as an alternation between cationic and anionic layers along the crystallographic b-axis. The dehydration of the precursor proceeds through three stages leading to crystalline intermediary hydrate phases and an anhydrous compound. The magnetic measurements show that the title compound is predominantly paramagnetic with weak antiferromagnetic interactions.     

Fabrication of β-Si3N4 whiskers by combustion synthesis with MgSiN2 as additives

β-Si₃N₄ whiskers with diameter of 0.5–2 μm and aspect ratio of 10–15 have been successfully prepared by combustion synthesis under 30–50 atm nitrogen pressure. The addition of MgSiN₂ powder plays a significant role in the growth of β-Si₃N₄ whiskers. The as-prepared products were characterized by X-ray powder diffraction (XRD) and scanning electron microscopy (SEM).     

Large-scale synthesis of ear-like Si3N4 dendrites from SiO2/Fe composites and Si powders

Large-scale ear-like Si₃N₄ dendrites were prepared by the reaction of SiO₂/Fe composites and Si powders in N₂ atmosphere. The product was characterized by field emission scanning electron microscopy, X-ray diffraction, and transmission electron microscopy. The results reveal that the product mainly consists of ear-like Si₃N₄ dendrites with crystal structures, which have a length of several microns and a diameter of 100-200 nm. Nanosized ladder-like Si₃N₄ was also obtained when changing the Fe content in the SiO₂/Fe composites. The Si₃N₄ nanoladders have a length of hundreds nanometers to several microns and a width of 100-300 nm. The ear-like Si₃N₄ dendrites are formed from a two-step growth process, the formation of inner stem structures followed by the epitaxial growth of secondary branches.