Thermogravimetric investigation of the effect of annealing conditions on the soft ferrite phase homogeneity

In the present work, the conventional method of increasing the efficiency of solid-phase synthesis of lithium–zinc ferrites that involves multiple intermediate grinding of briquetted reaction mixtures annealed at high temperatures is compared with a new radiation-thermal (RT) method using a high-power pulsed beam of accelerated electrons for heating of reaction mixtures. An analysis of the TG(M)/DTG(M) curves recorded in a magnetic field demonstrates that the efficiency of Li_0.3Zn_0.4Fe_2.3O₄ synthesis from Li₂CO₃–Fe₂O₃–ZnO mechanical mixture at a temperature of 700 °C during 120 min is equivalent to thermal annealing at 800 °C, but with the triple annealing duration.     

电化学方法分析铅阳极膜的相组成

本文提出使用线性电位扫描和电位衰退定性和定量分析铅在4.5mol·dm^-^3H2SO4(30℃)中形成的阳极膜的相组成并与现场X射线衍射, 原子吸收光谱, 阳极溶出等法比较。结果表明电位扫描伏安曲线的峰电位和电位扫描至峰电位左右时电极开路后, 所得的稳定电位可用于阳极膜相组成的定性分析, 电位扫描伏安电线电流峰的面积可用于阴极膜相组成的定量分析。本文的阳极膜由PbO·PbSO4, PbO2和PbOn(2>n>1)组成, 以PbO·PbSO4为主要成份。     

Influence of the phase behavior on the properties of ionic nanoemulsions prepared by the phase inversion composition method

The low-energy emulsification method phase inversion composition (PIC) was used to prepare O/W nanoemulsions in the W/oleylammonium chloride-oleylamine-C12E10/hexadecane ionic system, where the oleylammonium acted as a cationic surfactant. The results obtained, in terms of phase diagrams and emulsion characteristics, were compared with those obtained in the system W/potassium oleate-oleic acid-C12E10/hexadecane [I. Solè, A. Maestro, C. González, C. Solans, J.M. Gutiérrez, Langmuir 22 (2006) 8326], in which the oleate acted as an anionic surfactant. This study was done in order to extend the application range of the ionic nanoemulsions, not only in anionic systems but also in cationic ones, and in order to deep further into the nanoemulsion formation mechanism. The results show again that to obtain small droplet-sized nanoemulsions it is necessary to cross a direct cubic liquid crystal phase along the emulsification path, and it is also crucial to remain in this phase enough time and to use a proper mixing rate to incorporate all the oil into the liquid crystal. Then, when nanoemulsion forms, the oil is already intimately mixed with all the components, and the nanoemulsification is easier. Structural studies made with both cationic and anionic systems confirmed that the size of the "micelles" that form the cubic phase is the same or slightly smaller than the size of the nanoemulsion droplets obtained, depending on the emulsification path, which seems to point out that the nanoemulsions are formed in both cases by a dilution process of this cubic phase. When further watery solution is added to the cubic liquid crystal, these micelles separate, disrupting the cubic structure, and a small fraction of the surfactant migrates to the water. Moreover, due to the change in pH, the spontaneous curvature increases. Then, the phases in equilibrium are an oil-in-water microemulsion (W(m)) and the oil in excess. However, through this emulsification method, the surfactants can be "trapped" in a lower curvature than the spontaneous one, retaining all the oil nanoemulsified.     

Effects of vacuum annealing on the particle size and phase composition of nanocrystalline tungsten carbide powders

The effects of the vacuum annealing temperature (400–1400°C) on the phase and chemical composition, particle size, and microstresses of the nanocrystalline powders of tungsten carbide WC with 20–60 nm particles were studied by X-ray diffraction and electron microscopy. Vacuum annealing of WC nano-powders at T _ann ≤ 1400°C was accompanied by decarbonization, resulting from the interaction of carbon with the oxygen impurity. Changes in the chemical composition of the nanocrystalline powder of tungsten carbide led to changes in its phase composition. The annealing was accompanied by growth of powder particles due to the aggregation of nanoparticles and by a decrease of microstresses.     

Influence of pH of solution on phase composition of samarium-strontium cobaltite powders synthesized by wet chemical technique

Powders of Sm_0.6Sr_0.4CoO_3-δ and La_0.6Sr_0.4CoO_3-δ were synthesized using wet chemical technique. Structural and surface properties of synthesized materials were studied by thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), X-ray diffraction (XRD), IR spectroscopy, and scanning electron microscopy (SEM). The influence of pH on the phase state, chemical composition, morphology, and fractal dimension of the synthesized powders were investigated. It was found that the change of pH has the influence on phase composition of synthesized powders. The increase of solution pH allows one to obtain homogeneous samples at lower temperatures down to 900–950?°C.

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珍珠粉和贝壳粉的化学成分和结构特征分析

<正>珍珠粉是将珍珠贝壳动物马氏珠母贝、蚌科动物三角帆蚌或褶纹冠蚌等双壳动物受刺激形成的珍珠用物理的方法粉碎磨细而成的粉状物,自古以来就是名贵中药,具有安神定惊、明目消翳、解毒生肌之功效[1]。但是,市场上常出现以将蚌壳用碱去除其表面的角质层研细而成的贝壳粉,混充珍珠粉。查阅文献发现,由于珍珠粉和贝壳     

Preparation and some transformations of lithium-substituted acetals of the thiophene series

Some reactions of lithium-substituted acetals of the thiophene series are studied. It is shown that in reaction of some lithium thiophenes with 1-halogenopropynes there is an exchange reaction leading to the halogen atom being replaced by a lithium atom.     

New data obtained by thermomagnetometry,on the phase transitions in Ni,Co, Pt,Cu and Fe-C alloys

On the basis of thermomagnetic and DTA measurements, together with data from the literature, it may be concluded that in some f.c.c. metals a phase transformation occurs just before melting.

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Zusammenfassung Auf Grund thermomagnetischer und differentialthermoanalytischer Messungen sowie Literaturangaben wird geschlossen, dass in manchen kubisch-flächenzentrierten Metallen wenig unterhalb der Schmelztemperatur eine reversible Phasenumwandlung, wahrscheinlich in eine kubischraumzentrierte oder amorphe Phase, stattfindet.

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溶胶-凝胶法制备铁酸盐超微粒子催化剂

采用溶胶－凝胶法制备了含Zn,Ni,Co的铁酸盐超微粒子催化剂，运用DTA－TG、IR、XRD以及BET比表面测试等手段对所制备的样品进行了表征。同时，考察了铁酸盐对二氧化碳选择性氧化乙苯制苯乙烯的催化性能。结果表明：制备的铁酸盐均为尖晶石型晶体，粒子的比表面积为31．9－36．3m^2/g，晶粒大小约为30－35nm，在由二氧化碳选择性氧化乙苯制苯乙烯的反应中表现出较好的催化活性。     

Low sintering temperature of Mg-Cu-Zn ferrite prepared by the citrate precursor method

Mg-Cu-Zn ferrite was prepared through a wet synthetic method by a self-combustion reaction directly from a citrate precursor. The as-synthesized powders were sintered at 750 °C for only 2 h. XRD patterns and FTIR spectra confirm the formation of single phase Mg-Cu-Zn ferrite after combustion. To the best of our knowledge, this is the first time that Mg-Cu-Zn ferrite is sintered at such a low temperature. The sintering process increased the crystallinity of the solid and the domain sizes.     

Vacancy contents and phase equilibria of Ti-substituted MnZn ferrite

Measurement of the divalent iron content in acid dissolved MnZn ferrites, fired in controlled atmospheres at various temperatures and quenched, allows calculation of cation vacancy contents. Addition of Ti⁴⁺ to these ferrites resulted in the introduction of vacancies at the rate of about 0 to 0.3 per Ti⁴⁺ depending on heat treatment conditions. Data are presented whereby the vacancy content with Ti⁴⁺ can be calculated based on the oxygen content of the undoped ferrite as available in the literature. Ti⁴⁺ stabilizes the hexagonal hematite-like structure and the phase boundary is presented as a function of Ti⁴⁺ and temperature. The vacancy contents at the phase boundary in Ti⁴⁺-doped ferrite as a function of temperature are in agreement with those calculated from the literature for undoped MnZn ferrites. Finally, the total oxygen content of coexisting spinel and hexagonal phases is presented.     

Studies on the magnetism of cobalt ferrite nanocrystals synthesized by hydrothermal method

Fe-Co/CoFe₂O₄ nanocomposite and CoFe₂O₄ nanopowders were prepared by the hydrothermal method. The structure of magnetic powders were characterized by X-ray diffraction diffractometer (XRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), thermal gravity analysis (TGA) and differential thermal analysis (DTA) analysis, X-ray photoelectron spectrometry (XPS), and Fourier transform infrared spectra (FTIR) techniques, while magnetic properties were determined by using a vibrating sample magnetometer (VSM) at room temperature. The effects of hydrothermal reaction conditions on magnetic properties were also discussed in details. The values of saturation magnetization (M_s) and coercive fore (H_c) for Fe-Co/CoFe₂O₄ nanocomposite are 113 emu/g and 1.4 kOe, respectively. Furthermore, CoFe₂O₄ ferrite with a single-domain critical size of 70 nm was fabricated by controlling the hydrothermal reaction conditions carefully, which presents high coercive force (ca. 4.6 kOe) and high squareness ratio (ca. 0.65). One interesting thing is M_s value of CoFe₂O₄ ferrite with a diameter of 40 nm is 86 emu/g which is comparable to that of the bulk counterpart.     

Synthesis of ZnO:Ga nanosized powders by the combustion method

The synthesis of ZnO:Ga(0.075 wt%) nanosized powders via combustion reaction at 145°C and subsequent calcination of the ground combustion product at 500–900°C was studied. Zinc and gallium nitrates were used as initial substances, and sucrose, as fuel. It was found that Ga₂O₃ nanoparticles are located on the ZnO particles and inhibit their growth.     

Temperature effects on the composition and microstructure of spray-dried nanocomposite powders

Porous composite powders, prepared by spray drying of silica and polybromostyrene nanoparticles, were calcined at various temperatures up to 750 degrees C. The structure in these powders are quantitatively investigated by ultra small-angle X-ray scattering, thermogravimetric analysis, and nuclear magnetic resonance measurements. It has been found that the polybromostyrene latex is efficient in templating mesopores. However, polybromostyrene remains almost completely in the interstitial micropores in the grain after the spray-drying process. A post thermal treatment of the powders has been applied from 250 up to 750 degrees C. We found that the hydrocarbon part of the polybromostyrene is decomposed and leaves the micropores at around 350 degrees C. However, it is demonstrated that a significant amount of bromine remains in the interstitial micropores between the silica particles. At around 600 degrees C, the silica nanoparticles start to fuse with each other and a coalescence of the micropores takes place. At still higher temperature, around 750 degrees C, the micropore network totally disappears, and the growth in pore size occurs due to the coalescence of the mesopores with a significant decrease of the total porosity. During this process, the silica network densification is accompanied by a lowering of the specific surface area.     

Synthesis of Sr-doped LaCrO3 powders by combustion method

Lanthanum strontium chromite (LSC) powders were synthesized by the combustion method, using five different fuels (urea, glycine, ethylene glycol, ??-alanine, and citric acid). The ignition of the reagent mixture with urea takes a longer time, and more gases are released by combustion. A calcination step is essential for a good crystallization of the perovskite phase. X-ray diffraction patterns showed formation of perovskite phase and a small amount of SrCrO₄ for the sample synthesized with urea after calcination. The crystallite sizes are in the range of 23?C33?nm. Scanning electron microscopy revealed the porosity of the powders and the presence of agglomerates, formed by fine particles of different shapes. Thermogravimetric analysis showed a large mass loss for the sample synthesized with citric acid, probably caused by the absence of ignition, with primary polymerization of the precursor reagents.     

Analysis of the phase composition and an XRD study of industrial aluminum hydroxides

A quantitative phase analysis of aluminum hydroxides was performed by varying and optimizing parameters of the constituent crystalline phases so as to fit the measured and calculated XRD patterns. It was concluded that the system most probably consists of gibbsite crystalline structures and two pseudoboehmite forms.     

Morphology and structure of micro- and nanosize polytetrafluoroethylene powders prepared by the gas-phase method

Formation of fluoropolymer nanoaerosols and micropowders in the gas products of polytetrafluoroethylene pyrolysis and the hierarchical self-organization of ultradispersed powders were revealed. The features of the molecular and supramolecular structures of powders were analyzed. Low- and high-molecular-weight fractions of the fluoropolymers, constituting the powder particles were identified, and a method for their partitioning was proposed.     

Proton-exchanged waveguiding layers in Y-cut lithium niobate: Analysis of the phase composition by spectroscopic methods

A combination of methods was used for analysis of the phase composition of proton-exchanged layers in Y-cut lithium niobate. Mode spectra were used for the determination of phases. Vibration spectra allow some comparative and semi-quantitative estimations of the thickness of phase sub-layers to be made. The demonstrated method can contribute to adjustment of fabrication conditions for obtaining of defined phase compositions needed for waveguide devices with improved stability and characteristics.It was shown that deep and strongly protonated waveguides in Y-cut LiNbO₃ could be obtained at specific technological regimes.     

Synthesis of nanosized rubidium ferrite by thermolysis of ferricarboxylate precursors and combustion method

Nanosized pure rubidium ferrites have been successfully prepared by thermal decomposition of rubidium hexa(carboxylato)ferrate(III) precursors, Rb₃[Fe(L)₆]·xH₂O (L = formate, acetate, propionate, butyrate), in flowing air atmosphere from ambient temperature to 1000 °C. Various physico-chemical techniques i.e. simultaneous TG–DTG–DTA, XRD, Transmission Electron Microscope (TEM), IR and Mössbauer spectroscopy etc. have been employed to characterize the intermediates and end products. After dehydration, the anhydrous precursors undergo exothermic decomposition to yield various intermediates i.e. rubidium carbonate/acetate/propionate/butyrate and α-Fe₂O₃. A subsequent decomposition of these intermediates, followed by solid state reaction, lead to the formation of nanosized rubidium ferrite (RbFeO₂). The same nano-ferrite has also been prepared by the combustion method at a comparatively lower temperature and in less time than that of the conventional ceramic method (>1200 °C).     

The effects of electrolyte concentration on film composition and homogeneity in electrodeposition

We have investigated the effects of electrolyte concentration on the composition and homogeneity of thin films of the ternary alloy CoNiCu grown by single-bath electrodeposition techniques. The material was chosen owing to its academic and industrial applications but our results are more generic and will apply to other alloys grown this way. We compare weak (low species concentrations) and strong (high species concentrations) electrolyte solutions using identical electrolyte ratios. By choosing the concentration of the more noble species, in this case Cu, to be 25 times less than that of the other species, we controlled alloy composition as a function of potential. Films grown from the strong electrolyte solution were largely invariant in composition, whereas the weak solution produced highly potential sensitive alloy compositions. We found a trade-off between the accessible alloying range and thickness homogeneity across the film. This was shown to be due to the convective evolution of the diffusion layer using schlieren imaging.