Reaction sintering fabrication of (AlN, TiN)-Al2O3 composite

The (AlN, TiN)-Al₂O₃ composites were fabricated by reaction sintering powder mixtures containing 10-30 wt.% (Al, Ti)-Al₂O₃ at 1420-1520°C in nitrogen. It was found that the densification and mechanical properties of the sintered composites depended strongly on the Al, Ti contents of the starting powder and hot pressing parameters. Reaction sintering 20 wt.% (Al, Ti)-Al₂O₃ powder in nitrogen in 1520°C for 30 min yields (AlN, TiN)-Al₂O₃ composites with the best mechanical properties, with a hardness HRA of 94.1, bending strength of 687 MPa, and fracture toughness of 6.5 MPa m^1/2. Microstructure analysis indicated that TiN is present as well dispersed particulates within a matrix of Al₂O₃. The AlN identified by XRD was not directly observed, but probably resides at the Al₂O₃ grain boundary. The fracture mode of these composites was observed to be transgranular.     

Self-flux synthesis and photoluminescent properties of LiAl5O8

Pure-phase LiAl₅O₈ was selected as an oxide ceramic red phosphor material without dopants (color centers) and was synthesized using a self-flux method. The LiAl₅O₈ was formed by heating a powder mixture consisting of γ-Al₂O₃:Li₂SO₄ = 1:2 (molar ratio) at over 1100 °C for 1 h. Photoluminescence (PL) properties for the synthesized LiAl₅O₈ were investigated. The maximum intensity of the excitation spectrum for the photoluminescent emission of LiAl₅O₈ synthesized was at 274 nm. The peak intensity of the emission spectrum was at a wavelength of 667 nm (red color). The intensity of the peak emission spectrum increased with the heating temperature, i.e., the maximum peak intensity of the red emission spectrum was detected for the LiAl₅O₈ synthesized by heating at 1500 °C for 1 h.     

Preparation of flower-like CuO by a simple chemical precipitation method and their application as electrode materials for capacitor

A novel CuO electrode material with flower-like nanostructures was fabricated at a low temperature (80 °C) by a simple chemical precipitation method. Scanning electron microscopy (SEM) results showed that CuO with spherical and flower-like structure can be formed under a weak alkali (C₆H₁₂N₄), and CuO with sheets structure can be obtained under a strong alkali (NaOH). A possible growth mechanism of CuO nanocrystals was discussed. The flower-like CuO electrode exhibited a higher specific capacitance (133.6 Fg⁻¹) and an excellent cycle performance at a high current density of 10 mA/cm². Specific capacitance of flower-like CuO was 405.3% higher than globular CuO (26.44 Fg⁻¹) at 2 mA/cm².     

Synthesis of aluminum nitride powder by carbothermal reduction of a combustion synthesis precursor

A new homogeneous mixing precursor of alumina and carbon (Al₂O₃ + C) was prepared by low temperature combustion synthesis (LCS) with aluminum nitrate (Al(NO₃)₃·9H₂O), urea (CO(NH₂)₂), and glucose (C₆H₁₂O₆·H₂O) as starting materials. The precursor prepared was a foamy and porous mass due to the large amount of gases liberated in the combustion reaction and composed of nanosize particles. XRD analysis showed that this precursor consisted of amorphous alumina and carbon. The amorphous alumina in the precursor first transformed into γ-Al₂O₃, and then γ-Al₂O₃ was directly nitrided to yield AlN during the calcination process. The reaction temperature needed for a complete conversion for the precursor was about 1400 °C, which is much lower than that when using alumina and carbon black as starting materials. The synthesized AlN powder was composed of very fine particles and had good dispersability.     

Thermal decomposition of grinding activated bayerite

Bayerite [α-Al(OH)₃] was ground for 2 h and its structure change was characterized. Soft grinding reduces the grain size of bayerite, causes a lattice distortion in bayerite, and accelerates the phase transition from bayerite to the stable phases. With addition of α-Al₂O₃ seeds, calcining the ground bayerite at 300 °C leads to the onset of the α-Al₂O₃ formation. The onset temperature and the completion temperature of the transformation to α-Al₂O₃ in the ground bayerite are about 800 and 150 °C lower than the onset temperature and the completion temperature of the transformation to α-Al₂O₃ in the unground bayerite, respectively. The thermal decomposition of the ground bayerite undergoes the α-Al(OH)₃ → γ-AlOOH → γ-Al₂O₃ → α-Al₂O₃ path without the formation of the θ-Al₂O₃ transition phase. The effect of soft grinding on the structure of bayerite and the final thermal decomposition product of bayerite will be discussed.     

Effect of the fluoride additives on the oxidation of AlN

The oxidation of AlN powder added by the fluorides at temperatures below 700°C in air was discovered in this study. The obvious onset of oxidation of AlN with cryolite and YF₃ additions is below 700°C with the product of α-Al₂O₃ phase, which usually occurs in single AlN powder above 1100°C. The changes on the weight and the FTIR spectra of the AlN powder fired at temperatures lower than 700°C show that cryolite and YF₃ greatly promote the oxidation of AlN powder at these temperatures. Different from the action of cryolite and YF₃ powder, CaF₂ has no obvious effect on the oxidation of AlN. A possible oxidation process, in part corroborated by FTIR and XRF, was proposed to explain the results in the experiments. The oxidation kinetics of AlN in the presence of cryolite were also discussed at the temperatures ranging from 550 to 700°C from the data of the weight gains in this region. The result shows that the oxidation follows a linear law, which implies a reaction rate-controlled process. The considerably low activation energy of 67 kJ mol⁻¹, which is associated with the quick oxidation and the formation of α-Al₂O₃ at temperatures below 700°C, was determined from the slope of the line fit.     

Aluminium doped ceria–zirconia supported palladium-alumina catalyst with high oxygen storage capacity and CO oxidation activity

The Ce_0.5Zr_0.3Al_0.2O_1.9/Pd-γ-Al₂O₃ catalyst prepared by a mechanochemical route and calcined at 1000 °C for 20 h in air atmosphere to evaluate the thermal stability. The prepared Ce_0.5Zr_0.3Al_0.2O_1.9/Pd-γ-Al₂O₃ catalyst was characterized for the oxygen storage capacity (OSC) and CO oxidation activity in automotive catalysis. For the characterization, X-ray diffraction, transmission electron microscopy and the Brunauer–Emmet–Teller (BET) technique were employed. The OSC values of all samples were measured at 600 °C using thermogravimetric-differential thermal analysis. Ce_0.5Zr_0.3Al_0.2O_1.9/Pd-γ-Al₂O₃ catalyst calcined at 1000 °C for 20 h with a BET surface area of 41 m² g⁻¹ exhibited the considerably high OSC of 583 μmol-O g⁻¹ and good OSC performance stability. The same synthesis route was employed for the preparation of the CeO₂/Pd-γ-Al₂O₃ and Ce_0.5Zr_0.5O₂/Pd-γ-Al₂O₃ for comparison.     

Synthesis of submicron-sized spherical Y2O3 powder for transparent YAG ceramics

Spherical monodispersed, submicron-sized Y₂O₃ powder was prepared via a homogeneous precipitation method using nitrate and urea as raw materials. The structure, phase evolution and morphology of Y₂O₃ precursor and the calcined powder were studied by FTIR, TG/DTA, XRD and SEM methods. The sphere size of the precursor was about 250 nm and that of Y₂O₃ powder calcined at 800 °C for 2 h was about 200-210 nm. With the spherical Y₂O₃ powder and a commercial Al₂O₃ ultrafine powder, high transparent YAG ceramics was fabricated by vacuum sintering at 1780 °C for 6 h through a solid-state reaction method. The in-line transmittances of the as-fabricated YAG ceramics at the wavelength of 1064 nm and 400 nm were 82.8% and 79.5%, respectively, which were much higher than that of the YAG ceramics with a commercial Y₂O₃ powder and a commercial Al₂O₃ ultrafine powder directly. The superior properties are attributed to the good morphology, dispersibility and uniform grain size of the as-prepared spherical Y₂O₃ powder, which matches that of the commercial Al₂O₃ powder.     

Synthesis by an ionic liquid-assisted method and optical properties of nanoflower Y2O3

Flower-like Y₂O₃ nano-/microstructured phosphors without metal activators have successfully been fabricated by an ionic liquid (IL)-assisted method involving temperature (600 °C) annealing. In this paper, the effect of IL concentration on the morphology of the product has been investigated. The IL plays a crucial role in the formation of various morphologies of Y₂O₃. The structural and morphological features of the obtained samples have been characterized by means of X-ray powder diffraction (XRD) analysis, photoluminescence spectra (PL), Fourier-transform infrared (FT-IR) spectra and X-ray photoelectron spectra (XPS). The photoluminescence spectra of the products exhibit an intense bluish-white emission (ranging from 405 to 430 nm and centered at 418 nm). The luminescent mechanisms have been ascribed to the carbon impurities in the Y₂O₃ host. The effect of the ILs cation and the counter anions on the Y₂O₃ morphology of these nanostructures was studied experimentally. It was observed that Y₂O₃ morphology and PL of these nanostructures were strongly influenced by the type of cation and anion. As the length of the subsidiary chain of cation section of IL (imidaziole ione) reduces, the thickness of the nano-sheets increases. It is expected that the present method may easily be extended to similar nano-/microstructures of other oxide materials. Such investigations are currently underway.     

Hydrogen peroxide-assisted hydrothermal synthesis of hierarchical CuO flower-like nanostructures

Hierarchical CuO nanostructures were synthesized through a hydrogen peroxide-assisted hydrothermal route in which Cu(OH)₂ was the copper source. The CuO nanostructures were composed of numerous nanobelts that radiated from the center of the nanostructure and formed a flower-like shape with a diameter of 5-10 μm. The nanobelts had lengths of 2.5-5 μm and widths of 150-200 nm. The H₂O₂ concentration directly influenced the product morphology. As the concentration of H₂O₂ increased, the length and width of the nanobelts increased and the quantity of the nanobelts decreased. The possible formation mechanism of hierarchical CuO flower-like nanostructures was presented.     

Novel synthesis of lace-like nanoribbons of boehmite and γ-alumina by dry gel conversion method

Pure lace-like nanoribbons of AlOOH boehmite have been fabricated by an innovative dry gel conversion without the presence of catalysts and templates. Through steam-assisted crystallization at 200 °C for 48 h, the dried powder of amorphous aluminium hydroxide gel was transformed to lace-like nanoribbons in length of 1-2 μm and width about 100 nm as well as thickness of 5-6 nm. After calcination at 600 °C for 5 h, γ-Al₂O₃ was obtained and the morphology of lacelike was preserved.     

Synthesis and characterization of nanocrystalline La2Mo2O9 fast oxide-ion conductor by an in-situ polymerization method

A nanocrystalline La₂Mo₂O₉ powder was synthesized via the pyrolysis of polyacrylate salt precursor prepared by an in situ polymerization of the metal salts and acrylic acid. The pyrolysis behavior of the polymeric precursor was studied by thermal (TG/DTA) analysis. The obtained product was characterized by X-ray diffraction (XRD) and transmission electron microscope (TEM) analysis. The results revealed that the average particle size is ∼25 nm for La₂Mo₂O₉ with good crystallinity. The synthesized nanocrystalline La₂Mo₂O₉ powder showed good sinterability and reached ∼99% of theoretical density when sintered at 800 °C for 4 h. The La₂Mo₂O₉ sample sintered at 800 °C, yield good microstructure with improved conductivity value of about 0.12 S/cm at 800 °C.     

Low temperature pH dependent synthesis of flower-like ZnO nanostructures with enhanced photocatalytic activity

In the present study we have synthesized flower-like ZnO nanostructures comprising of nanobelts of 20 nm width by template and surfactant free low-temperature (4 °C) aqueous solution route. The ZnO nanostructures exhibit flower-like morphology, having crystalline hexagonal wurtzite structure with (0 0 1) orientation. The flowers with size between 600 and 700 nm consist of ZnO units having crystallite size of ∼40 nm. Chemical and structural characterization reveals a significant role of precursor:ligand molar ratio, pH, and temperature in the formation of single-step flower-like ZnO at low temperature. Plausible growth mechanism for the formation of flower-like structure has been discussed in detail. Photoluminescence studies confirm formation of ZnO with the defects in crystal structure. The flower-like ZnO nanostructures exhibit enhanced photochemical degradation of methylene blue (MB) with the increased concentration of ligand, indicating attribution of structural features in the photocatalytic properties.     

High sensitivity chlorine gas sensors using CdIn2O4 thick film prepared by co-precipitation method

Gas-sensing properties to dilute Cl₂ have been investigated for CdIn₂O₄ thick film sensors prepared by co-precipitation method. Cadmium nitrate and indium nitrate were mixed in de-ionized water. The 0.1 M NaOH was added to the mixed solution. The co-precipitate obtained was washed, filtered, dried, and calcined at 600-900 °C for 4 h. The CdIn₂O₄ sensor prepared using the powder calcined at 600 °C showed high sensitivity (S=R_g/R_a) to dilute Cl₂ at 250 °C. In particular, the CdIn₂O₄ sensor showed the sensitivity as high as 1200 even to 0.2 ppm Cl₂. The crystal structure and surface morphology were examined by means of X-ray diffraction (XRD) and scanning electron microscopy (SEM), respectively.     

Molten salt synthesis of ZnNb2O6 powder

Pure ZnNb₂O₆ powder was successfully prepared by the molten salt synthesis method using Nb₂O₅ and ZnO as raw materials and a mixture of NaCl and KCl as the solvent. The phase form and morphology of the prepared powder were characterized by X-ray diffraction and scanning electron microscopy. The effect of reacting temperature on phase formation was investigated. The results indicated that the single phase ZnNb₂O₆ powder can be obtained by the molten salt synthesis method at 600 °C, and the SEM photographs show that the grains of the powder are rod-like particles.     

Synthesis of nanocrystalline magnesium aluminate (MgAl2O4) spinel powder by the urea-formaldehyde polymer gel combustion route

Nanocrystalline MgAl₂O₄ spinel powder was synthesized by the urea-formaldehyde (UF) polymer gel combustion route. A transparent gel formed from magnesium nitrate, aluminium nitrate and UF after drying underwet self-sustained combustion when initiated with a burning splinter. The combustion product on calcinations at 850 °C formed MgAl₂O₄ spinel. Calcination of the combustion product resulted in particle coarsening. The powder obtained by planetary ball milling of the spinel had a median particle size of 1.58 μm. The spinel particles are agglomerates of nanocrystallites of size in the range 10-30 nm. The compacts prepared by uni-axial pressing of the spinel powder sintered to >99% TD at 1600 °C.     

Microstructural and electrical changes in nickel manganite powder induced by mechanical activation

Nickel manganite powder synthesized by calcination of a stoichiometric mixture of manganese and nickel oxide was additionally mechanically activated in a high energy planetary ball mill for 5-60 min in order to obtain a pure NiMn₂O₄ phase. The as-prepared powders were uniaxially pressed into disc shape pellets and then sintered for 60 min at 1200 °C. Changes in the particle morphology induced by mechanical activation were monitored using scanning electron microscopy, while changes in powder structural characteristics were followed using X-ray powder diffraction. The ac impedance spectroscopy was performed on sintered nickel manganite samples at 25 °C, 50 °C and 80 °C. It was shown that mechanical activation intensifies transport processes causing a decrease in the average crystallites size, while longer activation times can lead to the formation of aggregates, defects and increase of lattice microstrains. The observed changes in microstructures were correlated with measured electrical properties in order to define optimal processing conditions.     

Self-assembly of ZnO nanosheets into nanoflowers at room temperature

A singularity flower-like ZnO nanostructure was prepared on a large scale through a very simple solution method at room temperature and under ambient pressure in a very short time. The flower-like ZnO nanostructures were self-assembled by thin and uniform nanosheets, with a thickness of around 5 nm. X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HRTEM) were used to characterize the structure and morphology. The possible growth mechanism was discussed based on the reaction process. The blue shift in the UV-vis spectra of the ZnO nanostructures was also observed.     

Grain growth and microstructural evolution of yttrium aluminum garnet nanocrystallites during calcination process

An yttrium aluminum garnet (YAG) precursor precipitate was synthesized by urea method using yttria (Y₂O₃) and aluminum nitrate (Al(NO₃)₃·9H₂O) as raw materials. The fresh wet precipitate was dried by supercritical carbon dioxide (CO₂) fluid and the resulting powder was calcined at temperatures from 600 to 1600 °C. Crystallization of YAG was detected at 800 °C, and completed at 900 °C. HRTEM images of the YAG product obtained above 900 °C revealed crystallographically specific oriented attachment along the [1 1 2] direction. Based on the observation of the particle morphology a possible growth mechanism of YAG nanoparticles was presented. The fast increase on the average crystallite size of YAG at temperatures from 900 to 1300 °C is attributed to the crystallographically specific oriented attachment growth process. As the growth process proceeds at higher temperatures, oriented attachment based growth becomes less important because of the increase on particle size, and the self-integration assisted by the Ostwald ripening becomes dominant.     

Synthesis, morphology and optical properties of multi-pods Au/FeO(OH) and Au/Fe2O3 nanostructures

Multi-pods Au/FeOOH nanostructures were synthesized by a hydrothermal treatment of an aqueous solution of mixed micellar formed by gold nanoparticles, hexadecyltrimethyl ammonium bromide (CTAB), and (NH₄)₃[FeF₆] at 160 °C for 48 h and sequential calcined at 290 °C for 1.5 h, resulting in the formation of multi-pods Au/Fe₂O₃ nanostructures. The as-obtained products were characterized by powder X-ray diffraction, transmission electron microscopy, selected area electron diffraction, field emission scanning electron microscopy, and UV-vis spectroscopy. Surface plasmon resonance band of gold nanoparticles was observed in the multi-pods Au/FeOOH nanostructures. However, a similar behavior was not seen with multi-pods Au/Fe₂O₃ nanostructures. The critical role of F⁻ ions and CTAB molecules in the formation of FeO(OH) multipods and the probable mechanism of the formation of multi-pods Au/FeOOH and Au/Fe₂O₃ nanostructures were discussed.