Synthesis of Al2O3 matrix composites by reactive infiltration

Reactive infiltration of a NiO-base blended powder with molten aluminium was attempted at 1673 K in order to obtain Al2O3 matrix composites containing a dispersion of Al3Ni, AlNi and/or AlNi3. The NiO powder was barely infiltrated by the molten aluminium after a 3600 s holding time at 1673 K. A continuous layer of Al2O3 was observed to exist at the infiltration front, which prevented any further infiltration. TiB2 particles were added to the NiO powder in order to absorb the heat of reaction between NiO and aluminium. When the TiB2 particle content in the [NiO+TiB2] powder blend was greater than 20 vol%, spontaneous infiltration occurred completely. Thus, it was shown that the addition of the TiB2 particles assisted in the spontaneous infiltration. The specimens produced by the in situ reaction consisted of Al2O3, TiB2 and Al3Ni. Al3Ni was mainly located between the TiB2 and Al2O3. The effect of the TiB2 addition on the infiltration kinetics was to decrease the maximum attainable temperature caused by the exothermic reaction. This in turn prevented the formation of a continuous Al2O3 film at the infiltration front. This resulted in the production of pathways for the infiltration of the molten aluminium and made possible the complete infiltration. This revised version was published online in November 2006 with corrections to the Cover Date.     

Synthesis of spherical Al2O3 and AlN powder from C@Al2O3 composite powder

A novel approach has been taken to produce (1) spherical Al₂O₃ particles by decarbonisation and (2) spherical AlN particles by nitridation and subsequent decarbonisation of C@Al₂O₃ composite particles. C@Al₂O₃ composite particles have been prepared by heterogeneous nucleation and crystallisation of Al(NO₃)₃ on surfactant encapsulated carbon nano particles followed by evaporative decomposition of the nitrate. Overpressure (0.4 MPa) of nitrogen and a temperature range (1723–1873 K) have been used for nitridation. Whiskers as well as spherical particles of AlN have been observed in the final product. The final product has been characterised by X-Ray Diffraction, Scanning Electron Microscope and Carbon–Hydrogen–Nitrogen content analysis by Elemental Analyser and the mechanism of the nitridation reaction has been analysed. The average size of the spherical AlN particles consisting of crystallites in nano-dimensions (30–50 nm) could be varied from 100 nm to 8 μm by changing the composition of the sol.     

Synthesis of Al2O3-WC composite powder by SHS process

Al₂O₃-WC composite powder was synthesized by self-propagating high-temperature synthesis using Al powder as a reducing agent. WC, W₂C and Al₂O₃ were concurrently formed in WO₃-Al-C system. It was found that the complete reaction was achieved with excessive addition of carbon and appropriate processing parameters such as degree of dilution, particle size of aluminum, pellet compaction pressure and carbon source. The final product which was leached by 50% 1 : 4 HNO₃ + HF diluted solution was consisted of Al₂O₃-55wt%WC having 2–3 m of mean particle size.     

Synthesis of an Al2O3/Al co-continuous composite by reactive melt infiltration

The route for the fabrication of an Al₂O₃/Al co-continuous composite by reactive melt infiltration was investigated using scanning electron microscopy, energy dispersive X-ray microanalysis and X-ray diffraction analysis. It was found that in the process of molten aluminium infiltration into the SiO₂ preform, the chemical reaction of 3SiO₂ + 4Al → 2Al₂O₃ + 3Si occurred at the infiltration front, and generated a transition zone containing a new type of continuous porosity about 100 μm in width. The reaction continued with further infiltration of molten aluminium alloy into this porosity which reacted with the residual SiO₂ until all the SiO₂ was transformed into Al₂O₃. A comparison was made between this route and that by direct infiltration of molten aluminium alloy into the open porosity of an Al₂O₃ preform. As a result of the increased wetting ability of the molten aluminium alloy by the chemical reaction, reactive melt infiltration took place at a higher rate for the SiO₂ preform than that for the direct infiltration of the Al₂O₃ preform. A fracture surface examination demonstrated a toughening effect provided by the continuous aluminium alloy in the composite.     

Synthesis of hexagonal Al2−x Cr x O3 nanodisks by a thermal decomposition of mesoporous Cr4+:Al2O3 powders

Monodispersed hexagonal Al_2−x Cr _x O₃ nanodisks are synthesized through a reactive doping of Cr⁶⁺ cations in a hydrogenated mesoporous AlO(OH)·αH₂O powder followed by annealing at 1,200 °C in air. The reaction was carried out by a drop wise addition of an aqueous Cr⁶⁺ solution (0.5–1.0 M) to AlO(OH)·αH₂O, at room temperature. Al_2−x Cr _x O₃ nanostructure formation was controlled by the nucleation and growth from the intermediate amorphous mesoporous Cr⁴⁺:Al₂O₃ composites in the temperature range 400–1,000 °C. The nanodisks of ∼50 nm diameter and thickness of ∼16 nm is observed in the sample with x of 0.2 and similar nanodisks with a low dimension is observed at a higher value of x of 1.6 (after 2 h of heating at 1,200 °C). The Cr³⁺ ↔ Al³⁺ substitution, x ≤ 1.2, inhibits grain growth in small crystallites. The crystallites in x = 0.2 composition have 43 nm diameter while it is 15 nm in those with x = 1.2 composition.     

Formation of Ge nanocrystals in Al2O3 matrix

Ge nanocrystals were formed in Al2O3 matrix by implantation of Ge ions into sapphire (alpha-Al2O3) substrates and subsequent annealing. Diagnostic techniques, Raman spectroscopy, XRD, TEM, EDS, and SAED were employed to monitor and study formation of Ge nanocrystals and their evolution during heat treatments. TEM and EDS analysis revealed the diffusion of Ge ions into the substrate during annealing process. While Ge nanocrystals with mean sizes of 15 nm were observed in the heavily implanted region small nanocrystals with mean sizes of 4 nm were identified underneath this region. Some grains of transition aluminas were formed in the implanted region which was amorphized during the implantation. Extensive stress between the transition aluminas and sapphire matrices and its effects on the matrix were detected. The effect of stress on the Raman and XRD spectra of Ge nanocrystals was discussed.     

Synthesis and characterizations of Dy3+ doped Sr3Al2O6:Eu2+ powder phosphors through citric acid precursor

Sr₃Al₂O₆:Eu²⁺, Dy³⁺ phosphors were synthesized by the polymer precursor method. The X-ray powder diffraction patterns show that the samples have a cubic structure with a space group of Pa3. In the excitation spectrum, the phosphors show a wide absorption in the UV region from 250 to 450 nm, which corresponds to the crystal field splitting of the Eu²⁺ d-orbital. All the emission spectrum of Sr₃Al₂O₆:Eu²⁺, Dy³⁺ phosphors show the broad band emission peaked at about 518 nm, which can be ascribed to the typical 4f⁶5d¹ → 4f⁷ transitions of Eu²⁺ ions. And the best dopant concentration of Dy³⁺ ions for Sr₃Al₂O₆:2 mol%Eu²⁺, xDy³⁺ phosphors is 2 mol%. The excitation wavelengths have no influences on emission peaks, but have clear influences on emission intensities.     

Synthesis and characterization Y2O3:Eu3+ nanocrystals prepared via solvothermal refluxing route

Y₂O₃:Eu³⁺ nanocrystals were prepared via co-precipitation–solvothermal refluxing–calcination method using three kinds of organic solvents, propylene glycol, 1,3-butanediol and polyethylene glycol and yttrium chloride hexahydrate and europium chloride as starting materials. The Y₂O₃:Eu³⁺ nanocrystals with diameter of 20–50 nm prepared by refluxing in polyethylene glycol followed by calcinations at 800–1000 °C exhibited the strongest luminescence at 611 nm under the excitation wavelength of 254 nm than the reference sample prepared via conventional co-precipitation method. The photoluminescence spectra of the samples were recorded at room temperature. The effect of concentration of Eu³⁺ (Eu³⁺/Y³⁺ atomic ratio: 0.01–0.1) on the photoluminescence intensity was also investigated. The samples with the Eu³⁺/Y³⁺ atomic ratio of 0.07 exhibited the strongest emission at 611 nm and quenching effect was observed above 0.10.     

Al2O3 reinforced Al/Ni intermetallic matrix composite by reactive sintering

An aluminium-nickel reinforced Al₂O₃ particulate composite was fabricated by a powder metallurgy route, where 35wt% aluminium and 30wt% nickel powders were mixed with 35wt% Al₂O₃ particles and compacted at 548 MPa. Sintering was carried out at 850 °C, where the synthesis reaction was sustained by the transient liquid phase resulting from the exothermic reaction associated with the formation of intermetallic compounds, i.e. reactive sintering. The resultant microstructure was studied using X-ray diffraction (XRD) and scanning electron microscopy coupled with energy dispersive spectroscopy (SEM-EDS). It was found that the initial distribution of individual constituent powders affect the outcome of the reactive sintering and that the inward diffusion of aluminium in nickel was responsible for nickel aluminide formation.     

Synthesis of magnesium-modified mesoporous Al2O3 with enhanced catalytic performance for propane dehydrogenation

Magnesium (Mg)-modified mesoporous alumina with different type and content of Mg was prepared and then used as the support for platinum-tin catalyst in propane dehydrogenation. It was found that the property of Mg in Al₂O₃ varied with the way of the addition of Mg precursors. For the grafted Mg species, the connection between Al₂O₃ and Mg was increased by the forming of Mg–O–Al bonds in the inner surface of Al₂O₃ pore. While for the traditional impregnation, Mg was attached loosely to the outer Al₂O₃ surface by the aggregation of MgO. Moreover, modifying the internal framework of Al₂O₃ by suitable content of Mg can enhance the interaction between Sn and support, leading to more amounts of tin in their oxidized states, which was beneficial to enhance the interaction of Pt with SnO_x species. As a result, agglomerations of metallic particles were suppressed and the catalyst exhibited the best catalytic performance in terms of activity and stability.     

Hydrothermal synthesis of Eu3+-doped Y2Sn2O7 nanocrystals

Fine powders of Y₂Sn₂O₇ nanocrystals with pyrochlore structure have been successfully synthesized by the hydrothermal method in an alkaline system. The samples were characterized by X-ray diffraction, Fourier transform infrared and Raman spectroscopy. Furthermore, photoluminescence characterization of the Y₂Sn₂O₇ nanocrystals doped with 5 mol% Eu³⁺ was carried out, and the results show that there were some intense and prevailing emission peaks located at 580–635 nm.     

Structural and optical properties of ge nanocrystals embedded in Al2O3

Ge nanocrystals (NCs) embedded in aluminum oxide were grown by RF-magnetron sputtering. Raman, high resolution transmission electron microscopy (HRTEM), selected area diffraction (SAD), and X-ray diffraction (XRD) techniques confirmed good cristallinity of the NCs from samples annealed at 800 degrees C. The average NC size was estimated to be around 7 nm. Photoluminescence (PL) measurements show an emission related to the NCs. The temperature dependence of the PL confirms the confinement phenomenon in the Ge NCs.     

Synthesis and luminescence study of Eu3+ in Zn2SiO4 nanocrystals

The sol–emulsion–gel method is used for the preparation of Eu³⁺ doped Zn₂SiO₄ nanoparticles. The luminescence spectra at 613 nm (⁵D₀ → ⁷F₂) and lifetime of the excited state of Eu³⁺ ions doped Zn₂SiO₄ nanocrystals are also found to be sensitive to the concentration (0.25–2.5 mol%) of ions. In case of 1000 °C annealed sample (0.25 mol% Eu³⁺) showed the single component decay of 2.02 ms. However, with increasing the concentration the decay is biexponential. We attribute this to an inter-ion exchange interaction wherein the more rapid decay is due to pair or cluster formation and the longer-lived emission originates from isolated ions within the insulating host.     

Concentration quenching of Eu2+ in SrO · 6Al2O3 : Eu2+ phosphor

In SrO · 6Al₂O₃ : Eu²⁺ phosphor, blue Eu²⁺ luminescence is observed from Eu²⁺ on the strontium site present in the lattice. The concentration quenching process between Eu²⁺ ions is determined and the corresponding concentration quenching mechanism is verified as dipole-dipole interaction. The value of the critical transfer distance is calculated as 25 Å and its reliability is confirmed by using Dexter's theory on energy transfer.