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.     

Synthesis of β-Si3N4 whiskers by SHS

This paper presents the results of SHS of β-Si₃N₄ whiskers from silicon powders with α-Si₃N₄ as diluents under high nitrogen pressure. The effect of the addition of different amounts of Y₂O₃ on β-Si₃N₄ whisker synthesis has been investigated in detail. The results revealed that Y₂O₃ additive had a marked effect on the growth of β-Si₃N₄ whiskers compared that without additives. The optimum amount of Y₂O₃ addition is from 2.4 to 4.8 wt.%.     

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.     

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.     

Solution combustion synthesis of CeO2-CeAlO3 nano-composites by mixture-of-fuels approach

Nano-composites of CeO₂-CeAlO₃ are synthesised by solution combustion method employing (a) urea and (b) a mixture of urea and glycine as fuels with corresponding metal nitrates. The as-prepared powders are all nano-sized (5-30 nm) and the same is confirmed by broadening of the X-ray diffraction peaks and transmission electron microscopy. A starting composition of Ce:Al in the atomic ratio 4:6 gives rise to different phases depending on the fuel being used for combustion. When urea alone is used as fuel, nano-crystalline CeO₂ phase is formed with Al₂O₃ being in the amorphous state. When the mixture of fuels is used, a mixture of nano-sized CeO₂ and CeAlO₃ phases is obtained. However, upon sintering at 1400 ° C in air, the stable phases CeO₂ and -Al₂O₃ are formed in both the cases. Combustion synthesis using mixture-of-fuels is proposed to be a route to stabilise low oxidation compounds such as CeAlO₃.     

Lamellar Fe/Al2O3 catalyst for high-yield production of multi-walled carbon nanotubes bundles

The lamellar Fe/Al₂O₃ catalysts were prepared by sol-gel method, and then with these prepared catalysts, carbon nanotubes (CNTs) were synthesized by catalytic chemical vapor deposition (CCVD) method using C₂H₂ as precursor. The as-prepared CNTs and Fe/Al₂O₃ catalysts were characterized by X-ray diffraction, field emission scanning electron microscopy, transmission electron microscopy, high-resolution transmission electron microscopy and Raman spectrum. The results proved that the as-prepared CNTs actually existed in bundles. And the growth of CNTs bundles should be attributed to the lamellar catalysts, which supported the bottom growth mechanism of CNTs. The transition metal of Mo was not introduced in catalysts to produce CNTs bundles, which was different with others’ results.     

Morphological investigation of sub-micron FePO4 and LiFePO4 particles for rechargeable lithium batteries

Microstructural variations of amorphous FePO₄ and LiFePO₄ (the latter obtained by chemical lithiation of the former) as a result of the annealing temperature have been studied by Thermogravimetric Analysis (TGA)/Differential Thermal Analysis (DTA), chemical analysis, Brunauer-Emmet-Taylor (BET) and Scanning Electron Microscopy (SEM) techniques. Round-shaped amorphous FePO₄ particles 40-80 nm in size are obtained after heating (at 400 °C) amorphous FePO₄·2H₂O in air (previously prepared by a precipitation route). On further heating at 650 °C, in air, crystalline trigonal FePO₄ of crystallite size <200 nm is formed. Round-shaped amorphous LiFePO₄ particles 40-80 nm in size crystallize by heating at 550 °C in Ar+5%H₂ for 3 h. After thermal treatment, LiFePO₄ particles are interconnected by necks, which resembled a sintering process. The particle size of LiFePO₄ increases with an increase of temperature up to 750 °C, but an abnormal growth is evident at annealing temperatures above 650 °C. DTA analysis showed two exothermic peaks at 547 and 768 °C for FePO₄ due to phase transitions, whereas for LiFePO₄ two exothermic effects at 496 and 567 °C are shown.     

Controllable synthesis and magnetic property of BiMn2O5 crystals

Uniform submicron BiMn₂O₅ particles were prepared via a facile one-step hydrothermal route at low temperature. Bi(NO₃)₃, MnCl₂·4H₂O and KMnO₄ were used as starting materials; KOH as a pH adjustor and also as a mineralizer. Single-crystalline orthorhombic BiMn₂O₅ sample with controllable morphology was obtained. The microstructure strongly depends on the molar ratio of the starting materials, KOH concentration and reaction temperature. X-ray photoelectron spectroscopy shows the existence of Mn⁴⁺ state. Magnetic measurement indicates Néel temperature T_N at 44 K. The susceptibility above T_N obeys the Curie-Weiss law, χ = C/(T − θ), with θ = −350 K. The effective paramagnetic moment μ_eff = 4.66 μ_B/Mn, demonstrating the coexistence of mixed Mn³⁺ and Mn⁴⁺ valences.     

Bioactivity and mechanical properties of CaSiO3/high-density polyethylene (HDPE) composites prepared by a new surface loading method of CaSiO3 powder

CaSiO₃/high-density polyethylene (HDPE) composites with flexibility and biocompatibility were prepared by a new surface loading method. CaSiO₃ powder was synthesized by coprecipitation method with heating at 1300 °C for 2 h. The obtained α-CaSiO₃ powder was sieved to 45-75 μm (sample M) and 75-150 μm (sample C). Fine powder sample (sample F) was prepared by grinding the powder being the average particle size of 2.9 μm. These powders were sprinkled on the melted HDPE sheets heated at 160, 180 and 200 °C. The amounts of sprinkled powder were only <0.1 vol.% but the ratios of surface coverage area were >50% in all the samples. Apatite formation in simulated body fluid (SBF) was observed by soaking for 5 days in sample F while within 1 day in samples M and C. The sample M retained flexible properties of HDPE together with excellent biocompatible properties.     

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.     

Activated combustion features in the Mo-Si-C-promoter system and synthesis of MoSi2-SiC composite powders

Opportunities on combustion synthesizing the MoSi₂-SiC ceramic composites in a wide range of compositions under the chemical activated mode were studied. Molybdenum, silicon powders and carbon black were used as initial reagents, and Teflon was used as an activating additive. It was established that Teflon displays a dual (kinetic and thermal) impact on the interaction between reagents. The phasic character of the combustion process evolution, being characterized by low- and high-temperature regimes, was revealed. The end-products were subjected to SEM, XRD and chemical analyses.     

Fabrication and photocatalysis of mesoporous ZnWO4 with PAMAM as a template

Mesoporous ZnWO₄ was prepared with the template of PAMAM. The as-formed samples were characterized by X-ray diffraction (XRD), nitrogen absorption, scanning electron microscopy (SEM), transmission electron microscopy (TEM), and UV-vis diffuse reflectance spectroscopy (DRS). It is found that the size of pore is in the range of 5-22 nm and that the porosity of ZnWO₄ is composed of aggregated ZnWO₄ nanoparticles. The photocatalytic activities towards degradation of rhodamine B (RhB) and malachite green (MG) under UV light has been investigated. The formation mechanism of mesoporous structures is proposed.     

Preparation of Y2O3-Al2O3-SiO2 glasses by combustion synthesis melt-casting under high gravity

Y₂O₃-Al₂O₃-SiO₂ glasses were prepared by combustion synthesis melt-casting under high gravity. The properties of the glasses strongly depended on the starting compositions and preparation conditions. With a higher SiO₂ content in the starting compositions, the glass-forming ability of the melt was improved, but the density and hardness of the prepared glasses decreased. Crystallization occurred more frequently for larger samples and by using quartz crucibles instead of graphite ones. By increasing the high-gravity factors, both the density and hardness of the samples were improved. It is proposed that enhancing the high-gravity field facilitates the removal of bubbles from the melt.     

Facile synthesis of α-MnO2 nanostructures for supercapacitors

Various α-MnO₂ nanostructures have been successfully synthesized by a simple hydrothermal method based on the redox reactions between the MnO₄⁻ and H₂O in mixture containing KMnO₄ and HNO₃. The effect of varying the hydrothermal time to synthesize MnO₂ nanostructures and the forming mechanism of α-MnO₂ nanorods were investigated by using XRD, SEM and TEM. The results revealed an evolvement of morphologies ranging from brushy spherical morphology to nanorods depending upon the hydrothermal time. The surface area of the synthesized nanomaterials varied from 89 to 119 m²/g. Electrochemical properties of the products were evaluated using cyclic voltammetry and galvanostatic charge–discharge studies, and the sample obtained by hydrothermal reaction for 6 h at 120 °C showed maximum capacitance with a value of 152 F/g. In addition, long cycle life and excellent stability of the material were also demonstrated.     

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.     

In situ preparation of titanium matrix composites reinforced with TiB whiskers and Y2O3 particles

Titanium matrix composites reinforced with TiB and Y₂O₃ were prepared by a non-consumable arc-melting technology. X-ray diffraction (XRD) was used to identify the phases in the composites. Microstructures of the composites were observed by means of optical microscope (OM), scanning electron microscope (SEM), and transmission electron microscope (TEM). The results show that there are two kinds of reinforcements formed in the titanium matrix, needle-shaped TiB and Y₂O₃ with near-equiaxed and dendritic shape. The interfaces between reinforcements and titanium are clear and there is no evidence of interfacial reaction. The hardness of the composites decreases with the increasing contents of yttrium in the composite.     

Large-scale synthesis of ultralong Sb2S3 sub-microwires via a hydrothermal process

This paper describes an ethylene glycol (EG)-assisted approach to the large-scale ultralong Sb₂S₃ sub-microwires, formed by a simple hydrothermal reaction between SbCl₃ and Na₂S in the presence of distilled water. Transmission electron microscopy and scanning electron microscopy studies indicate that these Sb₂S₃ sub-microwires possess a diameter around 200 nm and length up to 100 μm. High-resolution transmission electron microscopy and selected area electron diffraction studies reveal that each Sb₂S₃ sub-microwire is a single-crystal along the [0 0 1] direction. The possible formation mechanism of the sub-microwires was discussed. The effects of volume ratio of EG/water, reaction temperature and the concentration of CO(NH₂)₂ on the morphology of Sb₂S₃ sub-microwires were also investigated.     

Combustion synthesis of TiCxN1−x-TiB2 ceramic composites in a high-gravity field

TiC_xN_1−x-TiB₂ ceramic composites were prepared by combustion synthesis in a high-gravity field in air. The high-gravity field caused no change in phase composition but resulted in reduced delamination and grain refinement in the microstructure of the products. In a high-gravity field of 100g, well-developed faceted grains with a narrow size distribution were obtained. It is proposed that the combustion reaction happened by a pulsating combustion mode and the pulsating period was prolonged by the high-gravity field.     

Pretreatment and sintering of Si3N4 powder synthesized by the high-temperature self-propagation method

Self-propagation high-temperature synthesis (SHS) was applied for the synthesis of low-cost Si₃N₄ powder. The powder was purified and ground until its particle size reached submicron levels and its purity reached 98%. Using this pretreated powder, with α/β = 60/40 content, fully dense Si₃N₄ ceramics, having improved mechanical properties, were obtained by liquid-phase sintering in the presence of (Y, La)₂O₃-AlN. The mechanical properties achieved finally were as follows: strength, 784 MPa; hardness, 15.1 GPa; and fracture toughness, 5.2 MPa m^0.5. The behaviors of the SHS-Si₃N₄ powders before and after the pretreatment were compared. The relation between microstructure and mechanical properties of the sintered specimens and the effect of different β content in the powder on the sintering process of Si₃N₄ were also studied.     

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.