Fabrication by Electrophoretic Deposition of Nano-Fe<Subscript>3</Subscript>O<Subscript>4</Subscript> and Fe<Subscript>3</Subscript>O<Subscript>4</Subscript>@SiO<Subscript>2</Subscript> 3D Structure on Carbon Fibers as Supercapacitor Materials

Core–shell nanostructured magnetic Fe₃O₄@SiO₂ with particle size ranging from 3 nm to 40 nm has been synthesized via a facile precipitation method. Tetraethyl orthosilicate was employed as surfactant to prepare core–shell structures from Fe₃O₄ nanoparticles synthesized from pomegranate peel extract using a green method. X-ray diffraction analysis, Fourier-transform infrared and ultraviolet–visible (UV–Vis) spectroscopies, transmission electron microscopy, and scanning electron microscopy with energy-dispersive spectroscopy were employed to characterize the samples. The prepared Fe₃O₄ nanoparticles were approximately 12 nm in size, and the thickness of the SiO₂ shell was?~?4 nm. Evaluation of the magnetic properties indicated lower saturation magnetization for Fe₃O₄@SiO₂ powder (~?11.26 emu/g) compared with Fe₃O₄ powder (~?13.30 emu/g), supporting successful wrapping of the Fe₃O₄ nanoparticles by SiO₂. As-prepared powders were deposited on carbon fibers (CFs) using electrophoretic deposition and their electrochemical behavior investigated. The rectangular-shaped cyclic voltagrams of Fe₃O₄@CF and Fe₃O₄@C@CF samples indicated electrochemical double-layer capacitor (EDLC) behavior. The higher specific capacitance of 477 F/g for Fe₃O₄@C@CF (at scan rate of 0.05 V/s in the potential range of ??1.13 to 0.45 V) compared with 205 F/g for Fe₃O₄@CF (at the same scan rate in the potential range of?~???1.04 to 0.24 V) makes the former a superior candidate for use in energy storage applications.     

Porous Y<Subscript>2</Subscript>O<Subscript>3</Subscript> microcubes: synthesis and characterization

In this work, a facile route using a simple solvothermal reaction and sequential heat treatment process to prepare porous Y₂O₃ microcubes is presented. The as-synthesized products were characterized by X-ray powder diffraction (XRD), scanning electronic microscope (SEM), energy dispersive spectrometer (EDS), thermogravimetric analysis (TG), and differential thermal analysis (DTA). The thermal decomposition process of the Y₂O₃ precursor was investigated. SEM results demonstrated that the as-prepared porous Y₂O₃ microcubes were with an average width of about 20 μm and thickness of about 8 μm. It was found that the morphology of the Y₂O₃ precursor could be readily tuned by varying the molar ratio of S₂O₈²⁻ to Y³⁺. Y₂O₃:Eu³⁺ (6.6%) microcubes were also prepared and their photoluminescence properties were investigated.     

Synthesis of ZSM-5 zeolite from metakaolinite: Effects of the SiO<Subscript>2</Subscript>/Al<Subscript>2</Subscript>O<Subscript>3</Subscript> molar ratio,the initial precursor and the presence of organic template agent

Highly crystalline ZSM-5 zeolites are successfully prepared from kaolinite as low cost precursor. The effects of SiO₂/Al₂O₃ molar ratio, the presence of tetrapropylammonium bromide (TPABr) and the initial precursor on the textural properties of the final products have been investigated. Crystallized samples have been characterized by scanning electron microscopy and nitrogen adsorption in addition to X-ray diffraction. The results show that getting pure ZSM-5 zeolite with a high crystallinity degree is directly dependent on the starting precursor as well as on the presence of the organic template highlighting the role of SiO₂/Al₂O₃ molar ratio. The directed-template ZSM-5 sample prepared frommetakaolinite with the smallest particles (crystal size of 700 nm) and a maximum crystallinity of 98% is obtained at a SiO₂/Al₂O₃ molar ratio of 31.69. Increasing the SiO₂/Al₂O₃ molar ratio to 41.13 isrequired to prepare an organic-template free ZSM-5 from metakaolinite with a relative crystallinity of 81%. In order to synthesize ZSM-5 zeolite from the acid-activated metakaolinite as the only silica and alumina sources, a SiO₂/Al₂O₃ molar ratio of 76.19 is used, the maximal crystallinity degree is 79%, with the largest ZSM crystals of about 3000 nm.     

Comparative analysis of the kinetics of dissolution of oxides Y<Subscript>2</Subscript>O<Subscript>3</Subscript> and Fe<Subscript>2</Subscript>O<Subscript>3</Subscript> in the iron matrix upon mechanical alloying

The kinetics of low-temperature dissolution of oxides Y₂O₃ and Fe₂O₃ in an iron matrix during mechanical alloying has been studied using electron microscopy. It has been shown that the dissolution rate upon deformation of primary coarse oxides Fe₂O₃ in α iron (and, hence, saturation of the α matrix with oxygen) during treatment in a ball mill for up to 10 h is several times higher than the dissolution rate of Y₂O₃ oxides. The high-temperature (1100°C) annealing of a mechanoalloyed mixture of Fe + 1.5% Y + 1.35% Fe₂O₃ leads to the precipitation of 60% (of the total number of particles) secondary oxides 2–5 nm in size and only of 5–7% secondary nanooxides in a mechanoalloyed mixture of Fe + 2% Y₂O₃.     

Luminescence properties of red-emitting Ca<Subscript>2</Subscript>Al<Subscript>2</Subscript>SiO<Subscript>7</Subscript>:Eu<Superscript>3+</Superscript> nanoparticles prepared by sol-gel method

A series of red-emitting Ca2-xAl2SiO7:xEu3+(x = 1 mol.%-10 mol.%) phosphors were synthesized by the sol-gel method.The effects of annealing temperature and doping concentration on the crystal structure and luminescence properties of Ca2Al2SiO7:Eu3+ phosphors were investigated.X-ray diffraction(XRD) profiles showed that all peaks could be attributed to the tetragonal Ca2Al2SiO7 phase when the sample was annealed at 1000℃.Scanning electron microscopy(SEM) micrographs indicate that the phosphors have an irregularly rounded morphology with particles of about 200 nm.Excitation spectra showed that the strong broad band at around 258 nm and weak sharp lines in 350-490 nm were attributed to the charge transfer band of Eu3+-O2-and f-f transitions within the 4f6 configuration of Eu3+ ions,respectively.Emission spectra implied that the red luminescence could be attributed to the transitions from the 5D0 excited level to the 7FJ(J = 0,1,2,3,4) levels of Eu3+ ions with the main electric dipole transition 5D0→7F2(618 and 620 nm),and Eu3+ ions prefer to occupy a lower symmetry site in the crystal lattice.Moreover,the photoluminescence(PL) intensity was strongly dependent on both the sintering temperature and doping concentration,and the highest PL intensity was observed at an Eu3+ concentration x = 7 mol.% after annealing at 1100℃.The obtained Ca2Al2SiO7:Eu3+ phosphor may have potential application for the red lamp phosphor.     

~ ~ 3＋ Sol-gel synthesis and photoluminescence characterization of La2Ti2O7.EU3＋nanocrystals

Eu³⁺ doped La₂Ti₂O₇ nanocrystals with pure monoclinic phase and size of about 100 nm were prepared by a citric acid (CA) assisted sol-gel method. Techniques of thermo-gravimetric (TG) and differential scanning calorimetry (DSC), X-ray diffraction (XRD), as well as transmission electron microscopy (TEM) were employed to characterize the as-synthesized nanoparticles. Furthermore, photoluminescence (PL) performances of the Eu³⁺ doped La₂Ti₂O₇ nanocrystals were evaluated with focus on the effects of calcination temperature and Eu³⁺ doping concentration on the photoluminescence properties.     

Preparation and characterization of nanostructured Bi<Subscript>2</Subscript>Se<Subscript>3</Subscript> and Sn<Subscript>0.5</Subscript>-Bi<Subscript>2</Subscript>Se<Subscript>3</Subscript>

Nanostructured Bi₂Se₃ and Sn_0.5-Bi₂Se₃ were successfully synthesized by hydrothermal coreduction from SnCl₂·H₂O and the oxides of Bi and Se. The products were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), and field emission scanning electron microscope (FESEM). Bi₂Se₃ powders obtained at 180°C and 150°C consist of hexagonal flakes of 50–150 nm in side length and nanorods of 30–100 nm in diameter and more than 1 μm in length. The product obtained at 120°C is composed of thin irregular nanosheets with a size of 100–200 nm and several nanometers in thickness. The major phase of Sn_0.5-Bi₂Se₃ synthesized at 180°C is similar to that of Bi₂Se₃. Sn_0.5-Bi₂Se₃ powders are primarily nanorod structures, but small amount of powders demonstrate irregular morphologies.     

Influences of NiCO<Subscript>3</Subscript> content on the microstructure and magnetic properties of Ni<Subscript>0.5</Subscript>Zn<Subscript>0.5</Subscript>Fe<Subscript>2</Subscript>O<Subscript>4</Subscript> powders prepared by SHS

Stoichiometric Ni_0.5Zn_0.5Fe₂O₄ powders were produced by self-propagating high temperature synthesis (SHS). The effects of NiCO₃ content in the raw materials on the microstructure and magnetic properties of Ni-Zn ferrite powders were systematically studied. The Ni_0.5Zn_0.5Fe₂O₄ powders were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The magnetic properties of the powders were evaluated by vibrating sample magnetometry (VSM). The results show that the introduction of NiCO₃ into reactants improves the conversion percentage and refines the Ni_0.5Zn_0.5Fe₂O₄ particles. The increase of NiCO₃ content enhances the magnetic properties of Ni_0.5Zn_0.5Fe₂O₄. Particularly, the saturation magnetization reaches the maximum when the NiCO₃ content is 3 at.%.     

Experimental Verification of the Decomposition of Y<Subscript>2</Subscript>O<Subscript>3</Subscript> in Fe-Based ODS Alloys During Mechanical Alloying Process

In this study, we investigated the state of Y₂O₃, as a major additive element in Fe-based ODS alloys, during mechanical alloying (MA) processes by thermodynamic approaches and experimental verification. For this purpose, we introduced Ti₂O₃ that formed different reaction products depending on the state of Y₂O₃ into the Fe-based ODS alloys. In addition, the reaction products of Ti₂O₃, Y, and Y₂O₃ powders were predicted approximately based on their formation enthalpy. The experimental results relating to the formation of Y-based complex oxides revealed that YTiO₃ and Y₂Ti₂O₇ were formed when Ti₂O₃ reacted with Y; in contrast, only Y₂Ti₂O₇ was detected during the reaction between Ti₂O₃ and Y₂O₃. In the alloy of Fe–Cr–Y₂O₃ with Ti₂O₃, YTiO₃ (formed by the reaction of Ti₂O₃ with Y) was detected after the MA and heat treatment processes were complete, even though Y₂O₃ was present in the system. Using these results, it was proved that Y₂O₃ decomposed into monoatomic Y and O during the MA process.     

Nanostructural Free-Volume Effects in Humidity-Sensitive MgO-Al<Subscript>2</Subscript>O<Subscript>3</Subscript> Ceramics for Sensor Applications

Technologically modified spinel MgO-Al₂O₃ ceramics were prepared from Al₂O₃ and 4MgCO₃·Mg(OH)₂·5H₂O powders at sintering temperatures of 1200, 1300, and 1400 °C. Free-volume structural effects in MgO-Al₂O₃ ceramics and their electrophysical properties were studied using combined x-ray diffraction, scanning electron microscopy, Hg-porosimetry, and positron annihilation lifetime spectroscopy. It is shown that increasing of sintering temperature from 1200 to 1400 °C results in the transformation of pore size distribution in ceramics from tri- to bi-modal including open macro- and meso(micro)pores with sizes from ten to hundreds nm and nanopores with sizes up to a few nm. Microstructure of these ceramics is improved with the increase of sintering temperature, which results in decreased amount of additional phases located near grain boundaries. These phase extractions serve as specific trapping centers for positrons penetrating the ceramics. The positron trapping and ortho-positronium decaying components are considered in the mathematical treatment of the measured spectra. Classic Tao-Eldrup model is used to draw the correlation between the ortho-positronium lifetime and the size of nanopores, which is complementary to porosimetry data. The studied ceramics with optimal nanoporous structure are highly sensitive to humidity changes in the region of 31-96% with minimal hysteresis in adsorption-desorption cycles.     

Effect of the addition of Sm<Subscript>2</Subscript>O<Subscript>3</Subscript> on the microstructure of laser cladding alloy coating layers

The effects on the microstructures and phases of coating layers by the addition of micron-sized (m) and nano-sized (n) (m&n) Sm₂O₃ powders were investigated. The coating materials, which were prepared by means of 2.0 kW CO₂ laser cladding, consist of a powder mixture of m Ni-based alloy (NBA) powders comprising 1.5 wt.% m Sm₂O₃ and 3.0% n Sm₂O₃ powders. The results indicate that γ-Ni, Cr₂₃C₆ and Ni₃B are the primary phases of the NBA coatings. The Fe₇Sm and Ni₃Si phases are highlighted by the addition of m&n Sm₂O₃ powders. From the substrate, planar crystal layers are first grown in all NBA and m&n Sm₂O₃/NBA coatings. The dendrite growth then occurs as a result of the addition of the m Sm₂O₃ powder, and the equiaxed dendrite growth occurs as a result of the addition of the n Sm₂O₃. With the addition of a rare earth oxide such as Sm₂O₃ powder, the width of the planar crystal becomes smaller than that of the NBA coating.     

Influence of Feedstock Powder Modification by Heat Treatments on the Properties of APS-Sprayed Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-40% TiO<Subscript>2</Subscript> Coatings

The formation and decomposition of aluminum titanate (Al₂TiO₅, tialite) in feedstock powders and coatings of the binary Al₂O₃-TiO₂ system are so far poorly understood. A commercial fused and crushed Al₂O₃-40%TiO₂ powder was selected as the feedstock for the experimental series presented in this paper, as the composition is close to that of Al₂TiO₅. Part of that powder was heat-treated in air at 1150 and 1500 °C in order to modify the phase composition, while not influencing the particle size distribution and processability. The powders were analyzed by thermal analysis, XRD and FESEM including EDS of metallographically prepared cross sections. Only a maximum content of about 45 wt.% Al₂TiO₅ was possible to obtain with the heat treatment at 1500 °C due to inhomogeneous distribution of Al and Ti in the original powder. Coatings were prepared by plasma spraying using a TriplexPro-210 (Oerlikon Metco) with Ar-H₂ and Ar-He plasma gas mixtures at plasma power levels of 41 and 48 kW. Coatings were studied by XRD, SEM including EDS linescans of metallographically prepared cross sections, and microhardness HV1. With the exception of the powder heat-treated at 1500 °C an Al₂TiO₅-Ti₃O₅ (tialite–anosovite) solid solution Al_2?xTi_1+xO₅ instead of Al₂TiO₅ existed in the initial powder and the coatings.     

Microstructure and Thermal Properties of Atmospheric Plasma-Sprayed Yb<Subscript>2</Subscript>Si<Subscript>2</Subscript>O<Subscript>7</Subscript> Coating

In the present work, Yb₂Si₂O₇ powder was synthesized by solid-state reaction using Yb₂O₃ and SiO₂ powders as starting materials. Atmospheric plasma spray technique was applied to fabricate Yb₂Si₂O₇ coating. The phase composition and microstructure of the coating were characterized. The density, open porosity and Vickers hardness of the coating were investigated. Its thermal stability was evaluated by thermogravimetry and differential thermal analysis (TG-DTA). The thermal diffusivity and thermal conductivity of the coating were measured. The results showed that the as-sprayed coating was mainly composed of crystalline Yb₂Si₂O₇ with amorphous phase. The coating had a dense structure containing defects, such as pores, interfaces and microcracks. The TG-DTA results showed that there was almost no mass change from room temperature to 1200 °C, while a sharp exothermic peak appeared at around 1038 °C in DTA curve, which indicated that the amorphous phase crystallized. The thermal conductivity of the coating decreased with rise in temperature up to 600 °C and then followed by an increase at higher temperatures. The minimum value of the thermal conductivity of the Yb₂Si₂O₇ coating was about 0.68 W/(m K).     

Phase Relations in the ZrO<Subscript>2</Subscript>-Nd<Subscript>2</Subscript>O<Subscript>3</Subscript>-Y<Subscript>2</Subscript>O<Subscript>3</Subscript> System: Experimental Study and Advanced Thermodynamic Modeling

Phase equilibria in the ZrO₂-Nd₂O₃-Y₂O₃ system at 1523-1873 K have been investigated by x-ray diffraction (XRD) and scanning electron microscopy combined with energy dispersive x-ray spectroscopy (SEM/EDX). Temperatures of phase transformations were determined by differential thermal analysis. Temperatures of invariant reactions in the ZrO₂-Nd₂O₃ system F = A + Pyr and H = F + A were determined as 1763 and 2118 K respectively and thermodynamic parameters of phases were re-assessed. Phase transformations in ternary systems were determined at 1732 K for composition ZrO₂-48.46Nd₂O₃-5.38Y₂O₃ (mol%) and at 1744 and 1881 K for composition ZrO₂-79.09Nd₂O₃-2.75Y₂O₃ (mol%). They were interpreted using XRD investigation before and after DTA as Pyr + B → F, Pyr → F and A → B, respectively. The solubility of the Y₂O₃ in pyrochlore phase was found to exceed 10 mol%. The thermodynamic parameters of the ZrO₂-Nd₂O₃-Y₂O₃ system were reassessed taking into account solubility of Y₂O₃ in the Nd₂Zr₂O₇ pyrochlore phase (Pyr). It is assumed that Y³⁺ substitutes Nd³⁺ and Zr⁴⁺ in their preferentially occupied sublattices. Ternary parameter was introduced into fluorite phase (F) for better reproducing of phase equilibria. Mixing parameters were reassessed for phase A (Nd₂O₃ based solution), monoclinic phase B and cubic phase C (Y₂O₃ based solution). The isothermal sections calculated for the ZrO₂-Nd₂O₃-Y₂O₃ system are in the reasonable agreement with experimental results.     

Cold spray of SiC and Al<Subscript>2</Subscript>O<Subscript>3</Subscript> with soft metal incorporation: A technical contribution

Al + SiC, Al + Al₂O₃ composites as well as pure Al, SiC, and Al₂O₃ coatings were prepared on Si substrates by the cold gas dynamic spray process (CGDS or cold spray). The powder composition of metal (Al) and ceramic (SiC, Al₂O₃) was varied into 1:1 and 10:1 wt.%, respectively. The propellant gas was air heated up to 330 °C and the gas pressure was fixed at 0.7 MPa. SiC and Al₂O₃ have been successfully sprayed producing coatings with more than 50 μm in thickness with the incorporation of Al as a binder. Also, hard ceramic particles showed peening effects on the coating surfaces. In the case of pure Al metal coating, there was no crater formation on hard Si substrates. However, when Al mixed with SiC and Al₂O₃, craters were observed and their quantities and sizes depended on the composition, aggregation and size of raw materials.     

Fabrication of Al matrix composite reinforced with submicrometer-sized Al<Subscript>2</Subscript>O<Subscript>3</Subscript> particles formed by combustion reaction between HEMM Al and V<Subscript>2</Subscript>O<Subscript>5</Subscript> composite particles during sintering

To fabricate an Al-V matrix composite reinforced with submicron-sized Al₂O₃ and Al_xV_y (Al₃V, Al₁₀V) phases, high energy mechanical milling (HEMM) and sintering were employed. By increasing the milling time, the size of mechanically milled powder was significantly reduced. In this study, the average powder size of 59 μm for Al, and 178 μm for V₂O₅ decreased with the formation of a new product, Al-Al₂O₃-Al_xV_y, with a size range from 1.3 μm to 2.6 μm formed by the in-situ combustion reaction during sintering of HEM milled Al and V₂O₅ composite powders. The in-situ reaction between Al and V₂O₅ during the HEMM and sintering transformed the Al₂O₃ and Al_xV_y (Al₃V, Al₁₀V) phases. Most of the reduced V reacted with excess the Al to form Al_xV_y (Al₃V, Al₁₀V) with very little V dissolved into Al matrix. By increasing the milling time and weight percentage of V₂O₅, the hardness of the Al-Al₂O₃-Al_xV_y composite sintered at 1173 K increased. The composite fabricated with the HEMM Al-20wt.%V₂O₅ composite powder and sintering at 1173 K for 2 h had the highest hardness.     

Mechanical synthesis and rapid consolidation of nanocrystalline 3Fe<Subscript>0.67</Subscript>Cr<Subscript>0.33</Subscript>-Al<Subscript>2</Subscript>O<Subscript>3</Subscript> composite by high frequency induction heating

Nanopowders of 3Fe_0.67Cr_0.33 and Al₂O₃ were synthesized from CrO₃ and 2FeAl powders by high-energy ball milling. A highly dense nanocrystalline 3Fe_0.67Cr_0.33-Al₂O₃ composite was consolidated by a high frequency induction heated sintering (HFIHS) method within three minutes from mechanically synthesized powders of Al₂O₃ and 3Fe_0.67Cr_0.33. The average grain size and mechanical properties of the composite were investigated.     

Properties and rapid low-temperature consolidation of nanocrystalline Fe-ZrO<Subscript>2</Subscript> composite by pulsed current activated sintering

Nanopowders of Fe and ZrO₂ were synthesized from Fe₂O₃ and Zr by high-energy ball milling. The powder sizes of Fe and ZrO₂ were 70 nm and 12 nm, respectively. Highly dense nanostructured 4/3Fe-ZrO₂ composite was consolidated by a pulsed current activated sintering method within 1 minute from the mechanically synthesized powders (Fe-ZrO₂) and horizontal milled Fe₂O₃+Zr powders under the 1 GPa pressure. The grain sizes of Fe and ZrO₂ in the composite were calculated. The average hardness and fracture toughness values of nanostuctured 4/3Fe-ZrO₂ composite were investigated.     

Phase Relations in the Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-V<Subscript>2</Subscript>O<Subscript>5</Subscript>-MoO<Subscript>3</Subscript> System in the Solid State. The Crystal Structure of AlVO<Subscript>4</Subscript>

Phase relations in the ternary oxide system Al₂O₃-V₂O₅-MoO₃ in the solid state in air have been investigated by using the x-ray diffraction (XRD) and differential thermal analysis/thermogravimetric (DTA/TG) methods. It was confirmed that in the subsolidus area of the Al₂O₃-V₂O₅-MoO₃ system, there exist seven phases, that is Al₂O₃, V₂O_5(s.s.), MoO₃, AlVO₄, Al₂(MoO₄)₃, AlVMoO₇, and V₉Mo₆O₄₀. Seven fields, in which particular phases coexist at equilibrium, were isolated. The crystal structure of AlVO₄ has been refined from x-ray powder diffraction data. Its space group is triclinic, , Z = 6, with a = 0.65323(1) nm, b = 0.77498(2) nm, c = 0.91233(3) nm, α = 96.175(2)°, β = 107.234(3)°, γ = 101.404(3)°, V = 0.42555 nm³. The crystal structure of the compound is isotypic with FeVO₄. Infrared (IR) spectra of AlVO₄ and FeVO₄ are compared.     

Cr<Subscript>3</Subscript>C<Subscript>2</Subscript>-NiCr HVOF-Sprayed Coatings: Microstructure and Properties Versus Powder Characteristics and Process Parameters

Two 75%Cr₃C₂-25%NiCr feedstock powders with the same size distribution but different production process were characterized and found quite different in terms of morphology and phase composition. The powders were sprayed in a HVOF Diamond Jet (Sulzer Metco DJ-2600) torch with five different values of the oxygen-to-hydrogen ratio in order to assess the influence of this parameter on the microstructure and properties of the coatings. The results show that the closed and dense microstructure of one powder (Woka 7302) results in coatings with lower amount of decarburization, less oxide formation and higher toughness compared to coatings from the other powder (Praxair 1375). It was found that the O₂/H₂ ratio impacts mainly on the Young’s modulus, which almost doubled by changing the ratio from 0.40 to 0.50, and on toughness, but does not notably affect the Vickers hardness.