In-situ fabrication of Al3V/Al2O3 nanocomposite through mechanochemical synthesis and evaluation of its mechanism

In this research, in situ fabrication of Al₃V based nanocomposite and its formation mechanism have been investigated. In order to synthesize Al₃V/Al₂O₃ nanocomposite, a mixture of Al and V₂O₅ powders was subjected to high-energy ball milling and the nanocomposite was produced through a mechanochemical reaction. The produced structure was isothermally heat-treated at 500–600 °C for 0.5–2 h under argon atmosphere. In order to evaluate the structural changes during milling and annealing, the synthesized powders were characterized by X-ray diffraction (XRD). Moreover, the powder morphological changes were studied by scanning electron microscopy (SEM). It was observed that the reaction between Al and V₂O₅ occurred after about 30 min and, the Al₃V and Al₂O₃ were formed in nanocrystalline structure with the continuing mechanical milling. Calculation of adiabatic temperature confirmed that reaction took place in combustion mode. In final stage of milling up to 40 h; it was observed that the Al₃V decomposed to Al and V so that the optimum time of milling to achieve fabrication of nanocomposite was determined to be about 20 h. Calculations based on Miedema’s model verified partial disordering of Al₃V during further milling and annealing of as-milled powder at 600 °C led to the ordering of Al₃V. The crystallite size of Al₃V and Al₂O₃ after annealing at 600 °C for 2 h remained in nanometer scale. So the final product appeared to be stable even after annealing.     

Mechanical properties of in-situ toughened Al2O3/Fe3Al

Mechanical properties of in-situ toughened Al₂O₃/Fe₃Al nano-/micro-composites were measured. Effects of Fe₃Al content, sintering temperature and holding time on properties and microstructure of the composites were investigated. The addition of Fe₃Al nano-particles decreased the aspect ratio and grain size of Al₂O₃, and changed the fracture mode of composites. The maximum bending strength and fracture toughness were 832 MPa and 7.96 MPa m^1/2, which were obtained in Al₂O₃/5 wt.% Fe₃Al sintered at 1530 °C and Al₂O₃/10 wt.% Fe₃Al sintered at 1600 °C, respectively. Compared to monolithic alumina, the strength increased by 132% and the toughness increased by 73%. The improvement in the mechanical properties of the composites was attributed to the change in fracture mode from intergranular fracture to transgranular fracture, the “in-situ reinforced effect” arising from the platelet grains of Al₂O₃ matrix, refined microstructure by dispersoids, as well as crack deflection and bridging of intergranular and intragranular Fe₃Al.     

Mechanochemical synthesis of Al2O3/Co nanocomposite by aluminothermic reaction

In this work, Al₂O₃/Co nanocomposite was successfully prepared by mechanochemical reaction between Co₃O₄ and Al powders in a planetary high energy ball mill. The mechanism of the reaction was dealt using X-ray diffraction (XRD), differential thermal analysis (DTA), and thermodynamics calculations. It was found that Co₃O₄ reacts with Al through a self-sustaining combustion reaction after an incubation period of 50 min and the reaction between Co₃O₄ and Al involves two steps. First, Co₃O₄ reacts with Al to form CoO and Al₂O₃ at the temperature around melting point of Al, and at higher temperature, CoO reacts with remaining Al to form Co and Al₂O₃. Mechanical activation process decreases the reaction temperature from 1041 °C for as-received Co₃O₄ and Al powder mixture to 869 °C for 45 min milled powders. After annealing of powder milled for 12 h, no phase transformation has been detected. The crystallite sizes of both α-Al₂O₃ and Co remained in nanometeric scale after annealing at 1000 °C for 1 h.     

Synthesis and characterization of Al (Al2O3–TiB2/Fe) nanocomposite by means of mechanical alloying and hot extrusion processes

Synthesis and characterization of Al–(Al₂O₃–TiB₂/Fe) nanocomposite by means of mechanical alloying and hot extrusion processes was the goal of this study. For this regards, mechanical alloying was done in two steps; formation of Al₂O₃–TiB₂/Fe reinforcements and preparation of Al-base nanocomposite. Results showed that Al₂O₃–TiB₂/Fe nanocomposite powders can synthesis by mechanical alloying and subsequent heat treatment at 700 °C. Hot extrusion of powder samples lead to preparation of fully dense Al-base nanocomposite. With increasing the amount of complex reinforcements, the compression strength was increased and reached to 560 MPa. Consolidated samples show good ductility related to the nature of Al₂O₃–TiB₂/Fe reinforcements.     

Structural and mechanical characterization of Al-based composite reinforced with heat treated Al2O3 particles

In this study, the addition of 1.00 wt.% Al₂O₃ crystals to the metal matrix of the liquid aluminum was studied. In order to investigate the influence of heat treatment on activation of Al₂O₃ powders and mechanical properties of Al–Al₂O₃ composites, the Al₂O₃ particles were heated at 1000 °C. X-ray Diffraction (XRD) analysis used to characterize the crystal lattice of Al₂O₃ and its variation during heat treatment. The size and morphology of the Al₂O₃ grains was evaluated by Scanning Electron Microscopy (SEM). The results showed a considerable change in morphology of Al₂O₃ grains during the heat treatment. Mechanical evaluation such as hardness, compression and wear tests showed enhancement in the properties of Al–1.00 wt.% heat treated Al₂O₃ vs. Al–1.00 wt.% Al₂O₃ composite.     

Improving the mechanical properties of Al2O3/Ni laminated composites by adding Ni particles in Al2O3 layers

The (Al₂O₃ + Ni) composite, (Al₂O₃ + Ni)/Ni and Al₂O₃/(Al₂O₃ + Ni)/Ni laminated materials were prepared by aqueous tape casting and hot pressing. Results indicated that the (Al₂O₃ + Ni) composite had higher strength and fracture toughness than those of pure Al₂O₃. The fracture toughness of (Al₂O₃ + Ni)/Ni and Al₂O₃/(Al₂O₃ + Ni)/Ni laminated materials was higher than not only those of pure Al₂O₃, but also those of Al₂O₃/Ni laminar with the same layer numbers and thickness ratio. It was found that the toughness of the Al₂O₃/(Al₂O₃ + Ni)/Ni laminated material with five layers and layer thickness ratio = 2 could reach 16.10 MPa m^1/2, which were about 4.6 times of pure Al₂O₃. The strength and toughness of the (Al₂O₃ + Ni)/Ni laminated material with three layers and layer thickness ratio = 2 could reach 417.41 MPa and 12.42 MPa m^1/2. It indicated the material had better mechanical property.     

Doping of iron phosphate glasses with Al2O3, SiO2 or B2O3 for improved thermal stability

The effects of doping 60 P₂O₅–40 Fe₂O₃ (mol%) glasses with 5–10 mol% SiO₂, Al₂O₃ or B₂O₃ on their thermal stability, iron environments and redox were investigated. Thermal stability improved markedly with 5% dopant addition in the order Al₂O₃ > SiO₂ > B₂O₃ ≫ base glass. Solubility of pro rata additions when melted at 1150 °C was 5–10% SiO₂, <5% Al₂O₃, and >10% B₂O₃. It was possible to dissolve 5% Al₂O₃ by replacing Fe₂O₃. These additions generally had little effect on dilatometric measurements and iron environments, however the Fe²⁺/ΣFe redox ratio increased in the order base glass < Al₂O₃ < SiO₂ < B₂O₃. This behaviour was broadly consistent with the effects of glass basicity. The increased thermal stability of these glasses may improve their suitability for applications such as waste immobilisation or sealing.     

Microstructure and mechanical properties of a directionally solidified Al2O3/Y3Al5O12/ZrO2 hypoeutectic in situ composite

Directionally solidified ternary Al₂O₃/Y₃Al₅O₁₂(YAG)/ZrO₂ hypoeutectic rod composites were successfully fabricated by the laser zone remelting technique. The microstructure and mechanical properties of the composite were investigated. The microstructure presented a complex three-dimensional network structure consisting of fine Al₂O₃ (41 vol.%) and YAG (49 vol.%) phases, with smaller ZrO₂ (10 vol.%) phases partially distributed at the Al₂O₃/YAG interfaces. The irregular growth behavior in the hypoeutectic was revealed. The hardness and fracture toughness at ambient temperature were measured to be 17.3 GPa and 5.2 MPa m^1/2, respectively. The toughness enhancement in comparison with previous binary Al₂O₃/YAG composites was mainly attributed to the refined microstructure, and crack deflection, branching and bridging. Moreover, the residual stresses, generated by different thermal expansion coefficients of the component phases, also importantly contributed to the improved toughness. Correlations between the addition of the third component ZrO₂ and the microstructure and properties were discussed as well.     

Phase transition of Er3+-doped Al2O3 powders prepared by the non-aqueous sol–gel method

The Er³⁺-doped Al₂O₃ powders have been prepared by the non-aqueous sol–gel method using the aluminum isopropoxide as precursor, acetylacetone as chelating agent, nitric acid as catalyzer, and hydrated erbium nitrate, as dopant under isopropanol environment. The phase structure and phase transition of the Er³⁺-doped Al₂O₃ powders were investigated by using thermogravimetry/differential thermal analysis (TG/DTA), Fourier transform infrared spectroscopy (FT-IR), and X-ray diffraction (XRD). The phase contents diagram for the Er-doped Al–O system with the doping concentration up to 5 mol% was described at the sintering temperature from 550 to 1250 °C. There were the three crystalline types of Er³⁺-doped Al₂O₃ phases, γ-, θ- and α-(Al, Er)₂O₃, and the two relative stoichiometric compounds composed of Al, Er, and O, ErAlO₃ and Al₁₀Er₆O₂₄ phases in the Er–Al–O phase contents diagram. The Er³⁺ doping suppressed crystallization of the γ and θ phases and delayed phase transition of the γ → θ and θ → α. The increased Er³⁺ doping concentration and the elevated sintering temperature enhanced the precipitation of the ErAlO₃ and Al₁₀Er₆O₂₄ phases. The preparation procedure for the Er³⁺-doped Al₂O₃ powders in the non-aqueous sol–gel process, including chelating, hydrolysis, peptization, doping and gelation, has a significant effect on the phase formation and its transition for the Er³⁺-doped Al₂O₃ powders.     

Sol–gel processing and phase characterization of Al2O3 and Al2O3/SiC nanocomposite powders

Monolithic Al₂O₃ and Al₂O₃/SiC nanocomposite powders were prepared by sol–gel processing. The process involved the precipitation of Al(NO₃)₃·9H₂O with NH₄OH in excess water to form boehmite (AlOOH). XRD indicates that the subsequent thermal reaction proceeds by the phase transformation sequence AlOOH, γ-, δ-, θ-, to α-Al₂O₃. The ²⁷Al NMR spectra indicate a gradual increase in the proportion of Al in the tetrahedral sites of the γ-, δ- and θ-Al₂O₃ formed at increasing calcination temperatures. Complete transformation to octahedral Al (α-Al₂O₃) is marked by the abrupt disappearance of tetrahedral Al. Al₂O₃/SiC nanocomposite powders were prepared by adding α-SiC powder to the boehmite precursor at the precipitation stage. Upon heating, the ²⁹Si NMR spectra of the Al₂O₃/SiC powders reveal α-SiC, Al₂O₃·xSiO₂ and SiO₂ phases. Stable α-Al₂O₃ and α-Al₂O₃/SiC nanocomposite powders are formed at 1200 and 1300 °C, respectively. It appears likely that the presence of SiC modifies the thermal behaviour of the Al₂O₃ in the nanocomposites by stabilising the Al₂O₃ phases with concomitant oxidation of SiO₂.     

Preparation of Al2O3–TiB2 nanocomposite powder by mechanochemical reaction between Al,B2O3 and Ti

Mechanochemical processing is a novel technique for the synthesis of nano-sized materials. This research is based on the production of Al₂O₃–TiB₂ nanocomposite powder using mechanochemical processing. For this purpose, a mixture of aluminum, titanium and boron oxide powders was subjected to high energy ball milling. The structural evaluation of powder particles after different milling times was conducted by X-ray diffractometry (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The results showed that during ball milling the Al/B₂O₃/Ti reacted with a combustion mode producing Al₂O₃–TiB₂ nanocomposite. In the final stage of milling, the crystallite sizes of Al₂O₃ and TiB₂ were estimated to be less than 50 nm.     

Mechanical properties of Al2O3/Ni laminated composites

Al₂O₃/Ni laminated composites were prepared by aqueous tape casting and hot pressing with intent to study mechanical properties including the fracture strength and toughness. The residual stress was evaluated and proved. The relations of mechanical properties with the thermal residual stress, the ductility of metal layers and the layer thickness ratio were studied, respectively. It was found that the toughness and work of fracture of Al₂O₃/Ni laminar reached to 12.56 MPa m^1/2 and 12 450 J m^− 2, which are 3.6 and 478.8 times that of pure Al₂O₃.     

Synthesis of Ti3AlC2/Al2O3 nanopowders by mechano-chemical reaction

Ti₃AlC₂/Al₂O₃ nanopowders were synthesized by the combination of mechanically-induce self-propagating reaction (MSR) of Ti, C, Al and TiO₂ powder mixtures and subsequently heat treatment. Effects of high energy milling and heat treatment temperatures on the phase transformation were investigated in detail. X-ray diffraction (XRD) was used to characterize the powders of milled and annealed, respectively. The morphology and microstructure of as fabricated products were also studied by scanning electron microscopy (SEM) equipped with energy-dispersive spectroscopy (EDS). Results show that TiC, Ti_xAl_y and Al₂O₃ transitional phases were formed when the initial powder mixtures were milled for 24 h. The desired Ti₃AlC₂/Al₂O₃ nanopowders with high purity were obtained when annealed the as-milled powders at 1100 °C. SEM image confirmed that the as fabricated Ti₃AlC₂/Al₂O₃ particles has nanocrystalline layered structural matrix of Ti₃AlC₂, and the second phase of nanosized Al₂O₃ disperses uniformly in the Ti₃AlC₂ matrix.     

Hot workability and deformation mechanisms in Mg/nano–Al2O3 composite

The response of extruded Mg/nano–Al₂O₃ (1 vol.%) composite to hot working in the temperature range 300–500 °C and strain rate range 0.0003–10 s^?1 has been characterized using processing map and kinetic analysis. The hot working window for the composite occurs at strain rates >0.1 s^?1 and the optimum range of temperature is 400–450 °C. In this window, the behavior of the composite is similar to that of the matrix and is controlled by the grain boundary self-diffusion. At lower strain rates, however, the composite exhibits much higher apparent activation energy than that for lattice self-diffusion unlike the matrix material. The deformed microstructures revealed that the prior particle boundaries decorated by the nano-Al₂O₃ particles, are stable and do not slide, rotate or migrate but kink after compressive deformation and as such contribute to the high temperature strength of the composite.     

Shear strength and wettability of active Sn3.5Ag4Ti(Ce,Ga) solder on Al2O3 ceramics

The work deals with the study of wettability of Sn3.5Ag4Ti(Ce,Ga) solder on ceramic material of Al₂O₃. The Sn3.5Ag4Ti(Ce,Ga) solder is used for ultrasonic soldering of metallic and ceramic materials. The microstructure of Sn3.5Ag4Ti(Ce,Ga) solder consists of a tin matrix, where non-uniformly distributed constituents of partially dissolved Ti and uniformly distributed fine needles of Ag–Sn phase were observed. The solder was of heterogeneous composition. X-ray diffraction analysis has revealed the presence of following phases: Ag₃Sn, Ti₆Sn₅, Ti₃Sn. For determination of melting point, the Differential scanning calorimetry analysis (DSC) was performed. Wettability of Sn3.5Ag4Ti(Ce,Ga) solder was determined at temperatures 800, 850 and 900 °C in dependence on wetting time. The best wettability of solder Θ = 46° was achieved at 850 °C/43 min. The experiments with high-temperature activation were performed in vacuum of 10^?4 Pa. On the basis of experience attained by measurement of contact angle, the soldered joints of Al₂O₃/Al₂O₃ and Al₂O₃/metal were fabricated in conditions of high-temperature activation in vacuum at temperature 850 °C/10 min. For comparison, also the joints fabricated in the conditions of ultrasonic activation in the air at temperature 280 °C/1 min were applied. The shear strength of joints of Al₂O₃/Al₂O₃ and Al₂O₃/metal fabricated with Sn3.5Ag4Ti(Ce,Ga) solder varied from 17 to 35 MPa. The shear strength of joints fabricated in vacuum is slightly higher than in the case of joints fabricated by use of power ultrasound.     

Al2O3–FeCrAl composites and functionally graded materials fabricated by reactive hot pressing

Al₂O₃–FeCrAl composites were fabricated by mixing Fe₂O₃, Al and Cr powders and then reactive hot pressing. The high temperature alloy FeCrAl was formed by the reaction of extra Al, Cr and the Fe reduced from Fe₂O₃. The Al₂O₃–FeCrAl composites with various Al₂O₃ fractions were successfully fabricated by the proper addition of extra Fe, Cr, Al or Al₂O₃ powders. A five-layer functionally graded material of YSZ–FeCrAl was fabricated using the Al₂O₃–FeCrAl composites with compositions of 25, 53.2 and 75 vol.% Al₂O₃ as interlayer. The results from XRD analysis, optical microscope observation and thermal cycling test show that the composites fabricated by this method consist of α-Al₂O₃ phase and (Fe, Cr, Al) solid solution. The α-Al₂O₃ grain formed by this in-situ reaction between Fe₂O₃ and Fe is ultrafine and uniform distribution. The three-point bending strength is 305.0 MPa for the composite with 53.2 vol.% Al₂O₃ prepared by the reactive hot pressing, about 20% higher than that of the composite with same composition prepared by ex situ hot pressing method (252.0 MPa). No cracking was found in the functionally graded materials after 10 thermal cycles up to 1000 °C due to the better metal–ceramic bond, continuous in microstructure at interface of FGM and good oxidation resistance component FeCrAl alloy formed in the FGM.     

Al2O3–TiO2 thin films on glass substrate by sol–gel technique

In the present research, self-cleaning Al₂O₃–TiO₂ thin films were successfully prepared on glass substrate using a sol–gel technique for photocatalytic applications. We investigated the phase structure, microstructure, adhesion and optical properties of the coatings by using XRD, SEM, scratch tester and UV/Vis spectrophotometer. Four different solutions were prepared by changing Al/Ti molar ratios such as 0, 0.07, 0.18 and 0.73. Glass substrates were coated by solutions of Ti-alkoxide, Al-chloride, glacial acetic acid and isopropanol. The obtained gel films were dried at 300 °C for 10 min and subsequently heat-treated at 500 °C for 5 min in air. The oxide thin films were annealed at 600 °C for 60 min in air. TiO₂, Ti₃O₅, TiO, Ti₂O, α-Al₂O₃ and AlTi phases were determined in the coatings. The microstructural observations demonstrated that Al₂O₃ content improved surface morphology of the films and the thickness of film and surface defects increased in accordance with number of dipping. It was found that the critical load values of the films with 0, 0.07, 0.18 and 0.73 Al/Ti molar ratios were found to be 11, 15, 22 and 28 mN, respectively. For the optical property, the absorption band of synthesized powders shifted from the UV region to the visible region according to the increase of the amount of Al dopant. The oxide films were found to be active for photocatalytic decomposition of methylene blue.     

Monocrystalline silicon surface passivation by Al2O3/porous silicon combined treatment

In this paper, we report on the effect of Al₂O₃/porous silicon combined treatment on the surface passivation of monocrystalline silicon (c-Si). Al₂O₃ films with a thickness of 5, 20 and 80 nm are deposited by pulsed laser deposition (PLD). It was demonstrated that Al₂O₃ coating is a very interesting low temperature solution for surface passivation. The level of surface passivation is determined by techniques based on photoconductance and FTIR. As a result, the effective minority carrier lifetime increase from 2 μs to 7 μs at a minority carrier density (Δn) of 1 × 10¹⁵ cm^?3 and the reflectivity reduce from 28% to about 7% after Al₂O₃/PS coating.     

Effect of cup and ball types on alumina–tungsten carbide nanocomposite powder synthesized by mechanical alloying

Alumina-based nanocomposite powders with tungsten carbides particulates were synthesized by ball milling WO₃, Al and graphite powders. X-ray Diffraction (XRD) was used to characterize the milled and annealed powders. Microstructures of milled powders were studied by Transmission Electron Microscopy (TEM). Results showed that Al₂O₃–W₂C composite formed after 5 h of milling with major amount of un-reacted W in stainless steel cup. The remained W was decreased to minor amount by increasing carbon content up to 10 wt.%. When milled with ZrO₂ cup and balls, Al₂O₃–W₂C composite was completely synthesized after 20 h of milling with the major impurity of ZrO₂. In the case of stainless steel cup and balls with 10 wt.% carbon, Fe impurity after 5 h of milling (maximum 0.09 wt.%) was removed from the powder by leaching in 3HCl·HNO₃ solution. The mean grain size of the powder milled for 5 h was less than 60 nm. The powder preserved its nanocrystalline nature after annealing at 800 °C.     

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.