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.     

Mechanochemical carboaluminothermic reduction of rutile to produce TiC–Al2O3 nanocomposite

This investigation aims to produce TiC–Al₂O₃ nanocomposite by reducing rutile with aluminum and graphite powder via a mechanochemical process. The effect of milling time on this process was investigated. The characterization of phase formation was carried out by XRD and SEM. Results showed that after a 10 h milling, the combustion reaction between Al, TiO₂ and C was started and promoted by a self-propagation high temperature synthesis. Extending the milling time to 20 h, the reaction was completed. The XRD study illustrated after a 20 h milling, the width of TiC and Al₂O₃ peaks increased while the crystallite sizes of these phases decreased to less than 28 nm. After annealing at 800 °C for 1 h in a tube furnace, TiC and Al₂O₃ crystallite sizes remained constant. However, raising the annealing temperature to 1200 °C caused TiC and Al₂O₃ crystallite size to increase to 49 nm and 63 nm, respectively. No new phase was detected after the heat treatment of the synthesised TiC–Al₂O₃ nanocomposite.     

Effect of 10Ce-TZP/Al2O3 nanocomposite particle amount and sintering temperature on the microstructure and mechanical properties of Al/(10Ce-TZP/Al2O3) nanocomposites

A zirconia/alumina nanocomposite stabilized with cerium oxide (Ce-TZP/Al₂O₃ nanocomposite) can be a good substitute as reinforcement in metal matrix composites. In the present study, the effect of the amount of 10Ce-TZP/Al₂O₃ particles on the microstructure and properties of Al/(10Ce-TZP/Al₂O₃) nanocomposites was investigated. For this purpose, aluminum powders with average size of 30 μm were ball-milled with 10Ce-TZP/Al₂O₃ nanocomposite powders (synthesized by aqueous combustion) in varying amounts of 1, 3, 5, 7, and 10 wt.%. Cylindrical-shape samples were prepared by pressing the powders at 600 MPa for 60 min while heating at 400–450 °C. The specimens were then characterized by scanning and transmission electron microscopy (SEM and TEM) in addition to different physical and mechanical testing methods in order to establish the optimal processing conditions. The highest compression strength was obtained in the composite with 7 wt.% (10Ce-TZP/Al₂O₃) sintered at 450 °C.     

A study on the mechanochemical behavior of TiO2–Al–Si system to produce Ti5Si3–Al2O3 nanocomposite

In the present study Ti₅Si₃–Al₂O₃ nanocomposite was synthesized by a displacement reaction between Al and TiO₂ in ball milling of TiO₂, Al and Si powders. The effect of milling time and heat treatment temperatures were also investigated. The structural changes of powder particles during mechanical alloying were investigated by X-ray diffraction (XRD). Morphology and microstructure of powders were characterized by scanning electron microscopy (SEM). It was found that after 10 h of MA, the reaction between Al and TiO₂ initiated in a gradual mode and after about 45 h of milling, the reaction was successfully completed. The final product consisted of Ti₅Si₃ intermetallic compound with a crystallite size of 13 nm and amorphous Al₂O₃. Heat treatment of this structure at 1050 °C led to the crystallization of Al₂O₃ and ordering of Ti₅Si₃. The crystallite size of Ti₅Si₃ and Al₂O₃ after annealing at 1050 °C for 1 h remained in nanometer scale. So the final product appeared to be stable upon annealing.     

Formation mechanism of NbSi2–Al2O3 nanocomposite subject to mechanical alloying

Silicide compounds such as NbSi₂ have many desirable properties such as high melting point, high resistance to oxidation and suitable electrical conductivity. However, they have limited practical use because of low ductility. To overcome this limit, we produced NbSi₂ based nanocomposite containing Alumina second phase by an exothermic reaction between Al and Nb₂O₅ in mechanical alloying of Al–Nb₂O₅–Si system. Structural and phase evolution throughout milling were investigated by using X-ray diffraction and microscopy methods. It followed that after 10 h of MA, the reaction between Al and niobium oxide began in a gradual mode and after around 40 h of milling; the reaction was successfully completed. The final product consisted of NbSi₂ intermetallic compound and nanocrystalline Al₂O₃ with a grain size of 15 and 45 nm, respectively. Microhardness and fracture toughness of nanocomposite were also measured which are greater than NbSi₂ intermetallic. As the result of this research we showed that high strength together with increased ductility could be gained in nanocomposite compounds.     

Nanocrystalline Al/Al12(Fe,V)3Si alloy prepared by mechanical alloying: Synthesis and thermodynamic analysis

Al–Al₁₂(Fe,V)₃Si nanocrystalline alloy was fabricated by mechanical alloying (MA) of Al–11.6Fe–1.3V–2.3Si (wt.%) powder mixture followed by a suitable subsequent annealing process. Structural changes of powder particles during the MA were investigated by X-ray diffraction (XRD). Microstructure of powder particles were characterized using scanning electron microscopy (SEM). Differential scanning calorimeter (DSC) was used to study thermal behavior of the as-milled product. A thermodynamic analysis of the process was performed using the extended Miedema model. This analysis showed that in the Al–11.6Fe–1.3V–2.3Si powder mixture, the thermodynamic driving force for solid solution formation is greater than that for amorphous phase formation. XRD results showed that no intermetallic phase is formed by MA alone. Microstructure of the powder after 60 h of MA consisted of a nanostructured Al-based solid solution, with a crystallite size of 19 nm. After annealing of the as-milled powder at 550 °C for 30 min, the Al₁₂(Fe,V)₃Si intermetallic phase precipitated in the Al matrix. The final alloy obtained by MA and subsequent annealing had a crystallite size of 49 nm and showed a high microhardness value of 249 HV which is higher than that reported for similar alloy obtained by melt spinning and subsequent milling.     

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.     

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 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.     

Influence of sol–gel derived Al2O3 film on the oxidation behavior of a Ti3Al based alloy

Al₂O₃ thin films were deposited on a Ti₃Al based alloy (Ti–24Al–14Nb–3V–0.5Mo–0.3Si) by sol–gel processing. Isothermal oxidation at temperatures of 900–1000 °C and cyclic oxidation at 800–900 °C were performed to test their effect on the oxidation behavior of the alloy. Results of the oxidation tests show that the oxidation parabolic rate constants of the alloy were reduced due to the applied thin film. This beneficial effect became weaker after longer oxidation time at 1000 °C. TiO₂ and Al₂O₃ were the main phases formed on the alloy. The thin film could promote the growth of Al₂O₃, causing an increase of the Al₂O₃ content in the composite oxides, sequentially decreased the oxidation rate. Nb/Al enriched as a layer in the alloy adjacent to the oxide/alloy interface in both the coated and uncoated alloy. The coated thin film decreased the thickness of the Nb/Al enrichment layer by reducing the scale growth rate.     

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.     

Synthesis of (Fe,Cr)3Al–Al2O3 nanocomposite through mechanochemical combustion reaction induced by ball milling of Cr,Al and Fe2O3 powders

In this work, (Fe,Cr)₃Al matrix nanocomposite reinforced by 47 vol.% Al₂O₃ was synthesized by mechanochemical reaction of Cr, 3Al and Fe₂O₃ powders mixture. The structural evaluation of powder particles during milling was done by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and differential thermal analysis (DTA). The results showed that at the early stage of milling, the thermite reaction between Fe₂O₃ and Al occurred and Fe and Al₂O₃ phases were formed. Then, the remaining Al and Cr were alloyed with Fe, leading to (Fe,Cr)₃Al–Al₂O₃ nanocomposite structure. Further investigations indicated that the presence of diluents (excess Al and Cr) did not change the modality of thermite reaction and the formation of (Fe,Cr)₃Al–Al₂O₃ nanocomposite proceeded with combustion process. The (Fe,Cr)₃Al–Al₂O₃ nanocomposite powder exhibited the hardness value of 1140 Hv which is significantly higher than 935 Hv obtained for (Fe,Cr)₃Al.     

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.     

Fabrication of Al2O3–20 vol.% Al nanocomposite powders using high energy milling and their sinterability

In this study, alumina-based matrix nanocomposite powders reinforced with Al particles were fabricated and investigated. The sinterability of the prepared nanocomposite powder at different firing temperature was also conducted. Their mechanical properties in terms of hardness and toughness were tested. Alumina and aluminum powder mixtures were milled in a planetary ball mill for various times up to 30 h in order to produce Al₂O₃–20% Al nanocomposite. The phase composition, morphological and microstructural changes during mechanical milling of the nanocomposite particles were characterized by X-ray diffraction (XRD), transmission electron microscope (TEM), scanning electron microscope (SEM) techniques, respectively. The crystallite size and internal strain were evaluated by XRD patterns using Scherrer methods.A uniform distribution of the Al reinforcement in the Al₂O₃ matrix was successfully obtained after milling the powders. The results revealed that there was no any sign of phase changes during the milling. The crystal size decreased with the prolongation of milling times, while the internal strain increased. A simple model is presented to illustrate the mechanical alloying of a ductile–brittle component system. A competition between the cold welding mechanism and the fracturing mechanism were found during powder milling and finally the above two mechanisms reached an equilibrium. The maximum relative density was obtained at 1500 °C. The harness of the sintered composite was decreased while the fracture toughness was improved after addition Al into alumina.     

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.     

Microstructural evolutions of nickel-aluminide nanocomposites during powder synthesis and thermal spray processes

The synthesis and microstructural evolutions of the NiAl-15 wt% (Al₂O₃–13% TiO₂) nanocomposite powders were studied. These nanocomposite powders are used as feedstock materials for thermal spray applications. These powders were prepared using high and low-energy mechanical milling of the Ni, Al powders and Al₂O₃–13% TiO₂ nanoparticle mixtures. High and low-energy ball-milled nanocomposite powders were also sprayed by means of high-velocity oxy fuel (HVOF) and air plasma spraying (APS) techniques respectively. The results showed that the formation of the NiAl intermetallic phase was noticed after 8 h of high-energy ball milling with nanometric grain sizes but in a low-energy ball mill, the powder particles contained only α-Ni solid solution with no trace of the intermetallic phase after 25 h of milling. The crystallite sizes in HVOF coating were in the nanometric range and the coating and feedstock powders showed the same phases. However, under the APS conditions, the coating was composed of the NiAl intermetallic phase in the α-Ni solid solution matrix. In both of the nanocomposite coatings, reinforcing nanoparticles (Al₂O₃–13% TiO₂) were located at the grain boundaries of the coatings and pinned the boundaries, therefore, the grain growth was prohibited during the thermal spraying processes.     

Fracture behaviour of α-Al2O3 ceramics reinforced with a mixture of single-wall and multi-wall carbon nanotubes

The extraordinary mechanical properties of single-wall carbon nanotubes (SWCNTs) and multi-wall carbon nanotubes (MWCNTs) have generated interest in incorporating them as toughening agents in ceramics. This work describes the fracture behaviour of an alumina (Al₂O₃) ceramic reinforced with a mixture of 0.05 wt% MWCNTs + 0.05 wt% SWCNTs. The CNT/Al₂O₃ nanocomposite was pressureless sintered in air using graphite powder as bed powder at 1520 °C for 1 h. The hardnesses and fracture toughnesses were lower than for pure Al₂O₃ and Al₂O₃ + 0.1 wt% SWCNTs and Al₂O₃ + 0.1 wt% MWCNTs. A predominantly transgranular fracture mode with a decrease in crack deflection and no pull-out was observed in the SWCNT + MWCNT–Al₂O₃ nanocomposite. MWCNTs had to the best reinforcing effect in Al₂O₃ nanocomposite.     

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.     

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.     

Properties of near- and sub-micrometre Al matrix composites strengthened with nano-scale in-situ Al2O3 aimed for low temperature applications

Mechanical and electrical properties of in-situ Al–Al₂O₃ metal matrix composites (MMCs) fabricated by powder metallurgy approach using different aluminium powders of particle size 0.8–21 µm and purity 99.8–99.996% were examined. Hot working powder consolidation by vacuum hot pressing at 270 °C and direct extrusion at 425 °C and reduction ratio of 7:1 were applied. Subsequently, extruded composite rods with the diameter of 7.5 mm were cold worked by groove rolling and rotary swaging to the wires with the diameter of 1.1 mm. Detailed microstructural characterization of composite materials was carried out. Stress-strain characteristics of composite wires were measured at 77 and 300 K. In addition, resistivity of all wires were measured by four-probe method between 25 and 300 K and eddy current losses at frequency 72 Hz and temperatures between 18 and 77 K. Obtained results clearly showed that properly designed Al–Al₂O₃ MMC materials can be utilized at low temperatures e.g., for the thermal stabilization of superconducting wires.