Simultaneous synthesis and consolidation of nanostuctured MgAl2O4 compound by high-frequency induction heated sintering

The rapid sintering of a nanostuctured MgAl₂O₄ compound in a short time was investigated with high-frequency induction heating sintering process. The advantage of this process is that it allows very quick densification to near theoretical density and prohibition of grain growth in nanostuctured materials. A highly dense nanostructured MgAl₂O₄ compound was produced with simultaneous application of 80 MPa pressure and induced current with output of total power capacity (15 kW) within 2 min. The sintering behavior, grain size, and mechanical properties of the MgAl₂O₄ compound were investigated.     

Mechanochemical synthesis and electrochemical properties of nanostructured electrode materials for Li ion batteries

We focus on the synthesis by ball milling and on the electrochemical characterization of nanocrystalline bimetallic and composite materials to be employed as anodes in Li ion batteries. Ni₃Sn₄ and Ni₃Sn₂ based compounds were obtained by ball milling of three different Ni–Sn mixtures. The properties of the resulting anodes for Li ion batteries were evaluated as a function of composition. Moreover, a biphasic system is presented, with CoSn₂ and CoSn type structures, arising from the synthesis of the Sn₃₁Co₂₈C₄₁ composition. When cycled in a Li cell, this material showed a high reversible specific capacity, about 450 mA h g⁻¹, and a very good electrochemical and structural stability, making it of interest for application purposes. Contribution to the Fall Meeting of the European Materials Research Society, Symposium D: 9th International Symposium on Electrochemical–Chemical Reactivity of Metastable Materials, Warsaw, 17th–21st September, 2007.     

Mechanochemical synthesis and properties of fullerene derivatives

A technique was developed of mechanochemical synthesis of the fullerene C₆₀ water-soluble derivatives. The derivatives obtained were characterized by elemental analysis, IR spectroscopy, and thermogravimetric analysis. The effect the substances obtained on the mechanical properties of the polyvinyl alcohol films was studied. A strengthening effect of fullerene derivatives on the elastic modulus, tensile strength, and tensile deformation of the polyvinyl alcohol films were found to become apparent already at the concentrations of 0.1–0.2 wt %.     

Mechanochemical synthesis of nanostructured fluorapatite/fluorhydroxyapatite and carbonated fluorapatite/fluorhydroxyapatite

Powder mixture of Ca(OH)₂-P₂O₅-CaF₂ were milled in planetary ball mill. A carbonated fluorhydroxyapatite, FHA Ca₁₀(PO₄)_1−y(CO₃)_y(PO₄)₅(OH)_2−2x1(F)_2x1 was formed after 5 h of milling and carbonated fluoroapatite Ca₁₀(PO₄)_1−y(CO₃)_y(PO₄)₅(F)₂ was formed after 9 h of milling. Complete transformation of the carbonated form of FA into then single phase of FA occurred after 9 h milling and thermally treating. The various experimental techniques like X-ray Diffraction (XRD), Differential Thermal Analysis (DTA), Infrared Spectroscopy (IR), Transmission Electron Microscopy and Scanning Electron Microscopy (SEM) were used to characterize the synthesized powders and to postulate reaction mechanisms’ steps- transformations of reactants involved.     

Rapid consolidation of nanostructured Ti from mechanically activated Ti and TiH<Subscript>2</Subscript> by pulsed-current activated sintering,and the mechanical properties of the product

Dense nanostructured Ti was sintered from mechanically activated Ti and TiH₂ powders by pulsed-current activated heating under a pressure of 80 Mpa. TiH₂ powder was decomposed to Ti during sintering. The hardness of the Ti increased, and the average grain size of the Ti decreased, with increasing milling time.     

Mechanochemical synthesis and some properties of dispersed lithium niobate

Interactions in the lithium carbonate-niobium pentoxide system upon mechanochemical treatment (MChT) in air and in water are studied. The products are examined using differential thermal and X-ray diffraction analyses; IR, Raman, and electron spectroscopy; nitrogen adsorption; and electron micros-copy. Activation of the reagents and direct mechanochemical synthesis of lithium metaniobate (LMN) were found to occur at 600–850 and 1000 rpm, respectively. Lithium metaniobate prepared by MChT has high dispersion, defect structure, and increased photocatalytic activity.     

Mechanochemical synthesis and crystal structure of alpha'-AlD3 and alpha-AlD3

AlD3 AlD3 was synthesized by ball milling of 3LiAlD4 + AlCl3. Planetary ball milling at room temperature resulted in a mixture of AlD3 (alpha and alpha') and Al in addition to LiCl, whereas cryomilling at 77 K resulted in only AlD3 and LiCl. The AlD3 obtained was a mixture of about 2/3alpha and 1/3alpha'. Alpha' was determined by powder neutron diffraction to take the beta-AlF3 structure with space group Cmcm and a = 6.470(3), b = 11.117(5), and c = 6.562(2) A. It is built up of corner-sharing AlD6 octahedra in an open structure with hexagonal holes of radius 3.9 A. Alpha' slowly decomposes during storage at 40 degrees C. Alpha-AlD3 is also described by a corner-sharing AlD6 network but in a more dense ReO3-type arrangement. Both AlD3 modifications have slightly shorter Al-D distances compared to Na3AlD6, Na2LiAlD6, and K2NaAlH6.     

Electroless synthesis of Ag nanoparticles on deposited nanostructured Si films

Two and three-dimensional Ag nanoparticle ensembles were synthesized on deposited nanostructured column-void Si films simply by film immersion into pure Ag(2)SO(4) or AgNO(3) solutions. In addition to functioning as a reducer, this nanostructured material provides immobilization and monodispersion of the Ag nanoparticles due to its systematic nanoscale topography. This is accomplished without the requirement of a surfactant, capping agent, or linker. Kinetics, as monitored from plasmon optical extinction, and infrared spectroscopy suggest accompanying oxide growth limits and finally inhibits synthesis enabling nanoparticle size control. Kinetics is also limited by Ag+ transport through the voids unless the Si film is ultrathin. Our synthesis approach offers significant advantages for surface-enhanced molecular detection, including the absence of any agents on the nanoparticle surfaces and the ability to obtain nanoparticle ensembles on any substrate.     

High-pressure synthesis and electrical properties of Mn3Ge5 with Mn11Si19-type structure

The new germanium-rich manganese germanide, Mn₃Ge₅, was synthesized at 600–1000°C and 4 GPa using a Belt-type apparatus. The crystal structure of Mn₃Ge₅ was identified as possessing the Mn₁₁Si₁₉ type with a tetragonal cell (Schoenflies symbolD_2d). The electrical resistivity of Mn₃Ge₅ increased with increasing temperature and saturated above 200 K. The thermoelectric power was 50–70 μV/K and its sign was positive. These data indicated that Mn₃Ge₅ was ap-type semiconductor or a semimetal.     

Si5H3,Si5H6,Si5Li3及Si5Na3原子簇结构的理论研究

利用Gaussian-94计算程序中的B3LYP方法，在6—311 G(2d)6d基组下，对Si5，Si5H3，Si5H6，Si5Li3和Si5Na33原子簇的几何结构进行优化和频率计算．结果表明，Si5原子簇中最稳定的具有D3h对称性的结构中，位于同一平面上的3个Si原子确实具有剩余的成键能力，可以与3个H，Li，Na原子和6个H原子形成稳定的化合物．研究还发现，虽然H，Li和Na都属同一主族，但它们与Si5原子簇中Si原子的键连方式却不同，而且它们的加入，对Si5原子簇的“三角双锥”结构也有不同的影响．     

Controllable synthesis and luminescent properties of three-dimensional nanostructured CaWO4:Tb3+ microspheres

Three-dimensional (3D) nanostructured CaWO(4):Tb(3+)microspheres assembled by submicrospindles were synthesized via a mild sonochemical route from an aqueous solution of CaCl(2), TbCl(3) and Na(2)WO(4) with the aid of surfactant Polyglycol 600 (PEG-600). The crystal structure and morphology of the as-prepared products were characterized by using X-ray diffraction (XRD) and field emission scanning electron microscopy (FE-SEM). Rietveld refinement was carried out on the XRD data. The results showed that the CaWO(4):Tb(3+)nanoparticles can be formed without ultrasonic irradiation or addition of PEG-600. With continuously increasing irradiation time the submicrospindles and microspheres could be self-assembled. The central diameter and length of the submicrospindles are around 190 and 500 nm, respectively. The 3D CaWO(4):Tb(3+)nanostructured microspheres with diameter of 2-4 μm were assembled by the submicrospindles. A possible formation mechanism for the 3D-structured CaWO(4):Tb(3+)microspheres was proposed. The Photoluminescent (PL) properties of Tb(3+) ions in the nanostructured CaWO(4) microspheres were studied. The energy transfer processes in CaWO(4):Tb(3+)microspheres were analyzed. The electric dipole-dipole energy transfers related to (5)D(3) level were studied by inspecting the fluorescence decay of (5)D(3) level. The energy transfer critical distance was estimated.     

The synthesis and properties of CaCu3Ti4O12 thin films

The CaCu₃Ti₄O₁₂ (CCTO) thin films were synthesized via a metal‐organic solution containing stoichiometric amounts of the metal cations at 700 °C for 1 h. The stable metal‐organic solution was prepared by dissolving calcium nitrate, copper nitrate, and tetrabuty titanate in grain alcohol. The phases, microstructures, and electric properties of CCTO thin films were characterized by X‐ray diffraction, scanning electron microscopy, atomic force microscope, and electric measurements. The results show that the CCTO thin films have homogeneous microstructure, smooth surface, low leakage current, and high values of dielectric constant. The low leakage current can be attributed to the small surface roughness. The high value of dielectric constant can be attributed to the internal barrier layer capacitor mechanism and metal‐insulator‐semiconductor junction of CCTO thin films. Copyright © 2013 John Wiley & Sons, Ltd.     

Mechanochemical synthesis of 5-acetylthiazole: A step toward green and sustainable chemistry

Mechanochemical synthesis of 5-acetylthiazole derivatives by one-pot three-component procedure over Silica Sulfuric acid under solvent-free conditions, has been developed. The durability of the catalyst was tested. The environmentally benign protocol introduced herein characterized by no hazardous organic solvent used, recyclability of the catalyst up to five runs without loss of its catalytic activity and high yields of products that confirm the utilization of some green chemistry principles in the mentioned protocol.     

Magnetic,transport and thermodynamic properties of Ce5Ni2Si3 compound

The magnetization M(T,H), specific heat C_p(T,H), electrical resistivity ρ(T), magnetoresistance MR(T,H), thermal conductivity κ(T) and thermopower S(T) measurements were performed on the antiferromagnetic compound Ce₅Ni₂Si₃ with the Néel temperature T_N = 5.7 K. The estimated effective moment μ_eff is close to the free ion value of Ce in its trivalent state. The negative sign of the paramagnetic Curie temperature θ_p indicate the antiferromagnetic nature of the magnetic ordering. The variation of magnetic resistivity ρ_mag with temperature in Ce₅Ni₂Si₃ can be explained by a competition of the crystal electric field (CEF) splitting, the Kondo effect and the magnetic order. Based on the thermopower and employing a simple single-ion Kondo model the Kondo temperature have been estimated. Magnetocaloric effect is small but shows a sign change, which may be caused by a metamagnetic behavior.     

Morphology,mechanical and thermal properties of composites of polypropylene and nanostructured wollastonite filler

Nanostructured wollastonite was synthesized by a sol–gel method and then used as a filler for polypropylene (PP). The obtained wollastonite particles were investigated using XRD, TEM and FTIR techniques. Non-isothermal crystallization measurements revealed that the wollastonite filler reduced the crystallization temperature of the matrix. TGA analyses showed improved thermal stability of the nanocomposite with respect to that of the pure polypropylene. From the DMA tan δ curves, it was concluded that the introduction of the filler into the PP matrix induced a slight shift of the β-transition (glass transition) towards higher temperature. The measurements of storage moduli showed that the nanocomposites have higher stiffness than the pure PP over the whole range of test temperature. An increase in stiffness was also confirmed by tensile measurements.     

溶胶-凝胶模板法制备BaTiO3纳米线及其光催化性能

纳米线为准一维纳米材料[1],因其具有优异的光学、电学及力学性能而引起人们的极大关注.它的制备方法有许多种,如分子束外延法、光刻法、CVD法、模板法[2]等.其中模板法由于具有实验装置简单,操作容易,形态可控,适用面广等特点而成为纳米材料合成领域的一大焦点.常用的模板有:有序空洞阵列氧化铝模板、含有孔洞无序分布的高分子模板、纳米洞孔玻璃模板.其中阳极氧化铝(AAO)模板具有孔径均一、排列有序、孔密度高、热稳定性好且孔径大小可控等优点,成为模板合成法中最常用模板之一[3].     

Mechanochemical synthesis of Na-β/β″-Al2O3

Na-β/β″-alumina powders were synthesized by a mechanochemical processing. The influences of mechanical activation in the phase composition and microstructure of the final powders were investigated. Fine Na-β/β″-alumina powders were obtained at a lower temperature than that of a conventional solid-state reaction processing. The mechanism of the mechanical activation was studied. It was found that mechanical activation greatly affected the calcining process and phase composition of the precursory powders.     

纳米Bi~2O~3微粒的固相合成及其电化学性能的研究

用室温和低温固相反应法,采用两种反应途径合成了纳米Bi~2O~3微粒,并用XRD,TEM,CV及恒流充放实验对其性能进行了研究。     

Polyanilme-montmorilltonite (PANl-MMT) nanocomposites: Mechanochemical synthesis,structure, thermostability and electrical properties

Polyaniline (PANI)-montmorillonite (MMT) nanocomposites were prepared by direct intercalation of aniline molecules into MMT galleries, followed by in situ mechanochemical polymerization under solvent free conditions. X-rays diffraction, Fourier Transform Infra Red analyses and UV-vis spectroscopy confirmed the successful synthesis of polyaniline chains between the MMT nano-interlayers. On increasing the amount of MMT basal spacing decreased gradually, suggesting less intercalation with decreasing amount of aniline. Scanning electron micrographs demonstrated strong differences between the morphologies of PANI-MMT nanocomposites and those of pure MMT and PANI. DC conductivity was measured in the temperature range from 145 K to 303 K using four probe methods. Temperature dependent DC conductivity of PANI and all the PANI-MMT composites followed 3 dimensional variable range hopping (3D VRH) model. Frequency dependent AC conductivity (σ_AC), dielectric constant (ɛ′) and loss factor (ɛ″) have been measured in the frequency range 10²–10⁶. All these measured quantities; σ_AC, ɛ′ and ɛ″ decreased with the increase in MMT content in the composites at all frequencies. The frequency dependence of σ_AC displayed a low frequency region below 10⁴ Hz with almost constant conductivity, while above this frequency a rapid rise in σ_AC was observed with a power law of frequency dependence with an exponent equal to 0.7. Both real and imaginary parts of the permittivity exhibited a low frequency dispersion which has been attributed to hopping of polarons and bipolarons in PANI and its composites. The thermal stability was checked by thermogravimetric analysis (TGA) and was found to be enhanced due to addition of MMT in the PANI.     

Mechanochemical synthesis and physical–chemical properties of carbon–fluorocarbon nanocomposition materials. A review

There are the described novel class of porous carbon–fluorocarbon nanocomposition materials “C–CF_1+x”, prepared via the mechanochemical activation (MA) in the heterogeneous mixed systems “nano-C–nano-CF_1+x”, having an atomic ratio C:F as 1.14–4.0. As nano-C it was used thermally expanded graphite TEG and mesoporous carbon material NUMS (free porosity 45–95% and specific area 25–400 m²/g). As nano-CF_1+x these were used a superstoichiometric fluorocarbons FS and FT (CF_1.18–1.25) having the coherent diffraction area (CDA) ∼20–25 Å, free porosity 60–70%, sum O + H₂O in mixtures ∼0.1–0.5 wt.%, and metals sum <0.01 wt.%.Prepared nanocomposites “C–CF_1+x” were studied by FTIR, Raman, XPS C1s, O1s, F1s, X-ray diffraction and by chemical C, H, F-analyses. It was shown, that decrease of weight in systems “C–CF_1+x” does not exceed 0.5 wt.% and stated two main features of the temporary dynamics in changes for all MA-products. These are monotonous changes in bulk properties, such as decrease of C-nanophase relative amounts, confirmed with XRD. Simultaneously, a decrease of sp³-C–F and sp³-CF₂-groups at 1200 and 1320 cm⁻¹ and an origination of sp³-C–F-groups at 1080–1120 cm⁻¹, typical for C₂F-like structures are observed. Decrease of specific surface is corresponding to decrease in CDA sizes and dencity for all MA-products.O-containing admixtures in starting materials have a key influence to interactions in nano-“C–CF_1+x” systems during MA-processing, despite to their low content. The main O-contained participant is H₂O and it is interaction with sp³-C–F–bonds is leading to primary hydrolytic substitution of F onto OH with the origin of surface sp³-C–OH-bonds and their subsequent transformations into edged sp²>CO or/and into ester bridges C–O–C among basal and edged nano-C and nano-fluorocarbon blocks. The presence of basal sp³-C–OH and edged sp²>CO (sp²>COOH)-groups is confirmed by FTIR and XPS C1s and O1s spectra for all MA-nanocomposites in “C–CF_1+x” systems. Changes in the surface properties of prepared MA-“C–CF_1+x” nanocomposites are corresponded to the origin of extrema in properties for MA-time 6–10 min, such as content of surface C-nanophases and surface F with the simultaneous appearance of extrema in the specific electro conductivities and capacitances. The nature of observed phenomena is explained by the origin of chemical carbon nanosized contacts on particle surface and it is possible to use for practical applications. The main difference among MA-“C–CF_1+x” nanocomposites is that the “FS–TEG” systems are dominated by sp²-C–sp³-C–F electroconductive bridges, whereas in “NUMS–FT” systems the character of conductivity is determined by contribution of ester bridges C–O–C.