Characterization of ultrafine La x Sr1−x MnO3 powder prepared by spray pyrolysis

The characterization of La _x Sr_1−x MnO₃ powders produced by spray pyrolysis using scanning electron microscopy (SEM) and transmission electron microscopy (TEM) observation, specific surface area (Brunauer-Emett-Teller), and particle size distribution measurements shows that the resultant large particles are loose agglomerates consisting of many small particles. However, the sintered tiny particles can form hard agglomerates, and the particle size increases remarkably. The structures of the powders before and after sintering were identified by x-ray diffraction (XRD). The study of the electrical property of the powder shows that the powder is a metallic conductor. In a reducing atmosphere, the powder can be decomposed. When the powder is cofired with yttria-stabilized zirconia 5% (YSZ) powder at 1200 °C for 5 h, no new phase is produced, and the powder remains a single provskite hexagonal-rhombohedral structure.     

Synthesis of Y2SiO5:Eu nanoparticles from a hydrothermally prepared silica sol

In this paper, a novel route for the synthesis of Y₂SiO₅ (YSO) nanoparticles doped with Eu³⁺ ions, based on the use of a hydrothermally prepared silica sol as a chemical precursor and nanostructuring template, is presented. X-ray powder diffraction revealed crystallization of nanoparticles in an X₁ monoclinic structural type (P2₁/c) with well pronounced diffraction peaks and without any sign of additional phases. Transmission electron microscopy showed that the particle diameter was around 40 nm and that the particles formed loose aggregates. The synthesized materials exhibited characteristic luminescence emission of the trivalent europium ion, with the strongest emission (⁵D₀ → ⁷F₂ transition) at 611.5 nm and a corresponding lifetime of 1.8 ms. Two site occupancy, as expected, were demonstrated.     

Lanthanum ferrite ferromagnetic nanocrystallites by a polymeric precursor route

Reactive lanthanum orthoferrite nanoparticles were obtained by a polymeric precursor route. Nanoparticle growth and crystallization from amorphous precursor, as well as the formation of a grain boundary network in polycrystalline aggregates at different calcination temperatures were studied by conventional and high-resolution electron microscopy; electron and X-ray diffraction analysis; Raman; IR; and UV-vis spectroscopy. Microstructure measurements were compared to X-ray diffraction and chemical analysis results. Electron diffraction, combined with electron microscopy results were used to determine the content of amorphous phase. The coherent crystalline domain size and the particle size have been monitored by XRD and electron microscopy in order to determine the evolution of both crystal size and the onset temperature for crystallites formation. The results demonstrate that at 550 °C we obtain pure single-phase nanocrystalline LaFeO₃, sized ∼40 nm, without the presence of amorphous phase. The magnetization curves in the 5-350 K range indicate weak ferromagnetism of the LaFeO₃ powders.     

Preparation of TiO<Subscript>2</Subscript> Nanopowders by Plasma Spray and Characterizations

TiO₂ powders with the range of 10-60 nm were prepared successfully by plasma spray in the self-developed plasma spray equipment. The prepared nanopowders were characterized by transmission electron microscopy, X-ray diffraction, and X-ray photoelectron spectroscopy. The results showed that the prepared TiO₂ nanopowders were the mixture of anatase phase and rutile phase, the main phase was anatase. There were O, Ti, and C elements in powders; Ti element still existed in tetravalent. The photocatalytic degradation of methyl orange indicated that all methyl orange (20 mg/L) can be degraded fully when the addition of prepared TiO₂ nanopowders and illumination time were 1 g/L and 150 min, respectively.     

Influence of partial substitution of Ge on crystallization kinetics, microstructure and magnetic property of Fe44Co44−xZr7B5Gex alloys

Partial substitution of Ge for Co in Fe₄₄Co₄₄Zr₇B₅ amorphous alloy is found to have a large influence on crystallization kinetics and magnetic property of the alloy. Activation energy of nanocrystallization of FeCo phase (primary crystallization) decreases by 90 kJ/mol with 4 at.% Ge substitution, while that of precipitations of Zr-type phase from a residual amorphous phase (secondary crystallization) increases by 106 kJ/mol. The suppression of the secondary crystallizations stabilizes the FeCo nanocrystals embedded in the residual amorphous phase for the Fe₄₄Co_44−xZr₇B₅Ge_x until higher temperatures. It is proposed that the stabilization mechanism is attributed to preferential partitioning of Ge in the residual amorphous phase revealed by scanning transmission electron microscopy analysis. Microstructure and coercivity for the annealed alloys are also presented in combination with the effect of the Ge substitutions.     

Thixoforming of AA 2017 aluminum alloy composites

A comparative evaluation has been carried out on the microstructure of aluminum based SiC and Al₂O₃ particle reinforced composites produced by semi-solid direct squeeze forming of composite powder at temperatures of 635-645 °C. The study is focused on the distribution of the reinforcement and the intermetallic phases, the porosity content, the microstructure of the matrix phase, the interfacial state and mechanical properties. The particle size of the reinforcements, the time of the high-energy ball milling procedure for the fabrication of composite powder and the semi-solid forming temperature had a strong influence on the quality of sample in terms of distribution of reinforcement and interfacial interaction. Ball milling improves the interface formation between reinforcement and matrix and influences the remelting behaviour. Increasing ball milling time and decreasing semi-solid forming temperature with isothermal holding time resulted in relatively homogenous microstructures and in a reduced amount of interaction between SiC and metal matrix. Best results were obtained for 5 vol.% SiC_p composites after 3 h ball milling, semi-solid formed at 635 °C and held for 10 min.     

Structure and electrochemical performance of FeF3/V2O5 composite cathode material for lithium-ion battery

Orthorhombic structure FeF₃ was synthesized by a liquid-phase method using FeCl₃, NaOH and HF solution as starting materials, and the FeF₃/V₂O₅ composites were prepared by milling the mixture of as-prepared FeF₃ and the conductive V₂O₅ powder. The properties of FeF₃/V₂O₅ composites were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), galvanostatic charge/discharge and cyclic voltammetry measurements. Results showed that the FeF₃/V₂O₅ composites can be used as cathode material for lithium-ion battery. Electrochemical measurements in a voltage range of 2.0–4.5 V reveal that the addition of conductive V₂O₅ improves significantly the electrochemical performance of FeF₃, and the FeF₃/V₂O₅ composite prepared by milling for 3 h exhibits high discharge capacity and good cycle performance, and its discharge capacity maintains about 209 mAh g⁻¹ at 0.1 C (23.7 mA g⁻¹) after 30 cycles.     

Synthesis-structure relations for reactive magnetron sputtered V2O5 films

V₂O₅ films were grown onto MgO (100) substrates by reactive magnetron sputtering between 26 °C to 300 °C to establish a detailed synthesis-structure relation. The effect of deposition temperature on structural characteristics and surface morphology was characterized using X-ray diffraction, Raman spectroscopy, atomic force microscopy and scanning and transmission electron microscopy. Films prepared at room temperature are amorphous while those deposited above 80 °C exhibit a polycrystalline structure with the orthorhombic symmetry of the V₂O₅ phase.     

Phase pure synthesis of BiFeO3 nanopowders using diverse precursor via co-precipitation method

Amorphous powder of BiFeO₃ (BFO) was synthesized at low-temperature (80 °C) by co-precipitation method. Optimal synthesis conditions for phase pure BFO were obtained. Powders were calcined in the temperature range from 400 to 600 °C for 1 h. Iso-statically pressed powder was sintered at 500 °C for 2 h. Differential scanning calorimetric thermo-gram guided for phase transition, crystallization and melting temperatures. X-ray diffraction confirmed the amorphous nature of as synthesized powder and phase formation of calcined powders. Calcination at temperature ≥400 °C resulted in nano crystalline powders with perovskite structure. Average crystallite size increased with the increase in calcination temperature. Scanning electron microscopic studies revealed dense granular microstructure of the sintered samples. The sintered samples exhibited high dc resistivity at room temperature which decreased with the increase in temperature. Dielectric constant, dielectric loss tangent and ac conductivity measurements were carried out in the frequency range (10 Hz to 2 MHz). The samples responded weak electric and magnetic polarization at room temperature with unsaturated and hysteresis free loops, respectively.     

Characterisation of HVOF sprayed Cr3C2-50(Ni20Cr) coating and the influence of binder properties on solid particle erosion behaviour

The coating Cr₃C₂ with 50 wt.% Ni20Cr deposited by high velocity oxy-fuel (HVOF) spray process was characterized in detail to investigate the effect of annealing on the solid particle erosion behaviour and understand the influence of the binder properties. Systematic characterization of the coating was carried out using electron microscopy (scanning electron microscopy (SEM), transmission electron microscopy (TEM) and electron probe microanalysis (EPMA)), X-ray diffraction (XRD), microindentation and nanoindentation techniques. The solid particle erosion tests were done on the as-sprayed coating and coatings annealed at 400 °C, 600 °C and 800 °C using silica erodent particles. The coefficient of restitution of the coated samples was also measured by WC ball impact tests to simulate dynamic impacts. The as-sprayed coating consisted of primary carbides and binder that was a mixture of amorphous and nanocrystalline phases. Annealing leads to recrystallisation of binder phase and precipitation of secondary carbides. The coating hardness and binder ductility change with annealing temperature. The erosion resistance improves with annealing up to 600 °C. In the as-sprayed coating, the amorphous phase, inter-splat boundaries and the elastic rebound characteristics affect the erosion response. While in the case of the coating annealed at 600 °C, the presence of ductile crystalline binder, fine carbide precipitates and embedment of erodent particles together improve solid particle erosion resistance.     

Kinetics and formation mechanism of amorphous Fe52Nb48 alloy powder fabricated by mechanical alloying

A single phase amorphous Fe₅₂Nb₄₈ alloy has been synthesized through a solid state interdiffusion of pure polycrystalline Fe and Nb powders at room temperature, using a high-energy ball-milling technique. The mechanisms of metallic glass formation and competing crystallization processes in the mechanically deformed composite powders have been investigated by means of X-ray diffraction, Mössbauer spectroscopy, differential thermal analysis, scanning electron microscopy and transmission electron microscopy. The numerous intimate layered composite particles of the diffusion couples that formed during the first and intermediate stages of milling time (0–56 ks), are intermixed to form amorphous phase(s) upon heating to about 625 K by so-called thermally assisted solid state amorphization, TASSA. The amorphization heat of formation for binary system via the TASSA, ΔH_a, was measured directly as a function of the milling time. Comparable with the TASSA, homogeneous amorphous alloys were fabricated directly without heating the composite multilayered particles upon milling these particles for longer milling time (86 ks–144 ks). The amorphization reaction here is attributed to the mechanical driven solid state amorphization. This single amorphous phase transforms into an order phase (μ phase) upon heating at 1088 K (crystallization temperature, T_x) with enthalpy change of crystallization, ΔH_x, of −8.3 kJ mol⁻¹.     

Synthesis of lanthanum carbonate nanoparticles via sonochemical method for preparation of lanthanum hydroxide and lanthanum oxide nanoparticles

Lanthanum carbonate nanoparticles were synthesized from the reaction of lanthanum acetate and Na₂CO₃ under sonication via sonochemical method. Lanthanum hydroxide nanoparticles were prepared by facial hydrothermal processing from the resulted product at 110 °C for 24 h. The role of surfactant, calcination temperature and sonication time were investigated on the morphology and particle size of the products. Products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectrum (XPS), and Fourier transform infrared (FT-IR) spectra. La₂O₃ nanoparticles were obtained by calcinations of the nanoparticles of lanthanum carbonate at 600 °C.     

In situ synthesis and characterization of polyaniline–CaCu3Ti4O12 nanocrystal composites

High dielectric constant (ca. 2.4 × 10⁶ at 1 kHz) nanocomposite of polyaniline (PANI)/CaCu₃Ti₄O₁₂ (CCTO) was synthesized using a simple procedure involving in situ polymerization of aniline in dil. HCl. The PANI and the composite were subjected to X-ray diffraction, Fourier transform infrared, thermo gravimetric, scanning electron microscopy and transmission electron microscopy analyses. The presence of the nanocrystallites of CCTO embedded in the nanofibers of PANI matrix was established by TEM. Frequency dependent characteristics of the dielectric constant, dielectric loss and AC conductivity were studied for the PANI and the composites. The dielectric constant increased as the CCTO content increased in PANI but decreased with increasing frequency (100 Hz–1 MHz) of measurement. The dielectric loss was two times less than the value obtained for pure PANI around 100 Hz. The AC conductivity increased slightly up to 2 kHz as the CCTO content increased in the PANI which was attributed to the polarization of the charge carriers.     

Mechanochemical synthesis of Al2O3-TiB2 nanocomposite powder from Al-TiO2-H3BO3 mixture

Alumina-titanium diboride nanocomposite (Al₂O₃-TiB₂) was produced using mixtures of titanium dioxide, acid boric and pure aluminum as raw materials via mechanochemical process. The phase transformation and structural characterization during mechanochemical process were utilized by X-ray diffractometry (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), and thermogravimetric analyses (TG-DTA) techniques. A thermodynamic appraisal showed that the reaction between TiO₂, B₂O₃ and Al is highly exothermic and should be self-sustaining. XRD analyses exhibited that the Al₂O₃-TiB₂ nanocomposite was formed after 1.5 h milling time. The results indicate that increasing milling time up to 40 h had no significant effect other than refining the crystallite size.     

The study of Li effect on the microstructure and tensile properties of cast Al-Mg2Si metal matrix composite

This study is undertaken to investigate the effect of different concentrations of Li (0.03-0.35%) on the microstructure and tensile properties of Al-15 wt.%Mg₂Si in situ metal matrix composite. The results showed that 0.15 wt.% Li addition changes the morphology of primary Mg₂Si from irregular or dendritic to polyhedral shape and its average particle size decreases from 32 μm to 4 μm. Microstructural observations also depicted that the morphology of the eutectic Mg₂Si phase alters from flake-like to coral-like. Further investigations on tensile tests revealed optimum Li level (0.15%) for improving both UTS and elongation values. A study of the fracture surfaces via scanning electron microscope (SEM) revealed a brittle mode of failure in unmodified composite however the addition of 0.15%Li converts the fracture behaviour to ductile. The behaviour is explained in terms of the presence of oxide bifilms in the liquid Al alloy.     

Production of nanoscale Ba(Zn1/3Nb2/3)O3 microwave dielectric ceramics by polymerised complex method

Ba(Zn_1/3Nb_2/3)O₃ nanoparticles have been synthesized by a polymerised complex method by using precursor materials of barium nitrate, zinc acetate, niobium oxide, hydrofluoric acid and citric acid. Thermal decomposition characteristics and crystallization behavior of the powders were investigated by the thermogravimetric and differential thermal analysis, X-ray diffractometer and Fourier transform infrared spectroscopy. Ba(Zn_1/3Nb_2/3)O₃ phase started to form at low temperature of 400 °C and, single phase Ba(Zn_1/3Nb_2/3)O₃ perovskite structure was obtained at 1000 °C. Microstructural investigation revealed that the major particle size of Ba(Zn_1/3Nb_2/3)O₃ nanoparticles were in the range of 80–110 nm with spherical morphology and homogeneous size distribution. But the powders also contained some agglomeration.     

反应等离子喷涂 Al2O3-TiB2-Al 复相涂层的反应机理

目的在铝合金表面制备Al2O3-TiB2-Al复合涂层,研究Al,TiO2,B2O3在等离子喷涂中的反应机理。方法采用反应等离子喷涂技术在铝合金表面制备复合涂层,应用扫描电镜与X射线衍射技术测试复合涂层的物相组成和显微组织,并通过燃烧波淬熄试验分析等离子喷涂产物。结果机械球磨可以有效降低粉末发生反应的活化能,等离子喷涂最佳飞行距离范围为150~200 mm。结论喷涂粉末在飞行过程中发生反应,经历了预热、熔化、分解、团聚等过程,验证了最终引燃发生燃烧化学反应的机理。     

Microstructural, thermal and magnetic properties of amorphous/nanocrystalline FeCrMnN alloys prepared by mechanical alloying and subsequent heat treatment

Amorphous FeCrMnN alloys were synthesized by mechanical alloying (MA) of the elemental powder mixtures under a nitrogen gas atmosphere. The phase identification and structural properties, morphological evolution, thermal behavior and magnetic properties of the mechanically alloyed powders were evaluated by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), differential scanning calorimetry (DSC) and vibrating sample magnetometer (VSM), respectively. According to the results, at the low milling times the structure consists of the nanocrystalline ferrite and austenite phases. By progression of the MA process, the quantity and homogeneity of the amorphous phase increase. At sufficiently high milling times (>120 h), the XRD pattern becomes halo, indicating complete amorphization. The results also show that the amorphous powders exhibit a wide supercooled liquid region. The crystallization of the amorphous phase occurs during the heating cycle in the DSC equipment and the amorphous phase is transformed into the crystalline compounds containing ferrite, CrN and Cr₂N. The magnetic studies reveal that the magnetic coercivity increases and then decreases. Also, the saturation magnetization decreases with the milling time and after the completion of the amorphization process (>120 h), the material shows a paramagnetic behavior. Although the magnetic behavior does not considerably change by heating the amorphous powders up to the crystallization temperature via DSC equipment, the material depicts a considerable saturation magnetization after the transformation of the amorphous phase to the nanocrystalline compounds.     

TiO2-g-C3N4 composite materials for photocatalytic H2 evolution under visible light irradiation

In this investigation, we report the preparation of TiO₂-g-C₃N₄ composite materials with varying the wt.% of g-C₃N₄, the characterization of these materials by various techniques and photocatalytic hydrogen production under visible light irradiation in the presence of methanol. The X-ray powder diffraction (XRD) shows that the composite materials are consist of anatase TiO₂ and g-C₃N₄. Fourier transform infrared (FT-IR) spectra show that the absorbance band intensity of composite materials was stronger than that of C₃N₄. The UV-vis absorption spectra show that the absorption edge of the composite materials shifts to the lower energy region comparing to pure anatase and to longer wavelengths with increasing the amount of C₃N₄. The significant photoluminescence quenching was observed in TiO₂-C₃N₄ composite materials, indicating the charge transfer from C₃N₄ to TiO₂. The visible light induced H₂ evolution rate was remarkably enhanced by coupling TiO₂ with C₃N₄.     

Electroless ternary Ni-W-P alloys containing micron size Al2O3 particles

In the present investigation electroless ternary NiWP-Al₂O₃ composite coatings were prepared using an electroless nickel bath. Second phase alumina particles (1 µm) were used to codeposit in the NiWP matrix. Nanocrystalline ternary NiWP alloys and composite coatings were obtained using an alkaline citrate based bath which was operated at pH 9 and temperature at 88 ± 2 °C. Mild steel was used as a substrate material and deposition was carried out for about 4 h to get a coating thickness of 25 ± 3 µm. Metallographic cross-sections were prepared to find out the coating thickness and also the uniform distribution of the aluminum oxide particles in NiWP matrix. Surface analysis carried out on both the coatings using scanning electron microscope (SEM) showed that particle incorporation in ternary NiWP matrix has increased the nodularity of composite coatings compared to fine nodular NiWP deposits. Elemental analysis of energy dispersive X-ray (EDX) results showed that codeposited P and W elements in plain NiWP deposit were 13 and 1.2 wt.%, respectively. There was a decrease in P content from 13 to 10 wt.% with a marginal variation in the incorporated W (1.01 wt.%) due to the codeposition of aluminum oxide particles in NiWP matrix. X-ray diffraction (XRD) studies carried out on as-plated deposits showed that both the deposits are X-ray amorphous with a grain size of around 3 nm. Phase transformation studies carried out on both the coatings showed that composite coatings exhibited better thermal stability compared to plain NiWP deposits. From the XRD studies it was found that metastable phases such as NiP and Ni₅P₂ present in the composite coatings heat treated at major exothermic peak temperature. Annealed composite coatings at various temperatures revealed higher microhardness values compared to plain NiWP deposits.