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.     

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.     

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.     

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.     

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.     

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.     

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.     

Study on preparation and mechanical property of nanocrystalline NiAl intermetallic

Nanocrystalline NiAl materials were fabricated using mechanical alloying and hot-pressing sintering technique. The crystal structural and microstructure of milled powders during mechanical alloying, and the microstructure and mechanical properties of bulk NiAl intermetallic were characterized. The results show that B2 ordered nanocrystalline NiAl powders were successfully synthesized by solid-state diffusion via the gradual exothermic reaction mechanism during mechanical alloying. Scanning electron microscope image confirmed that the powder particles were flat and flake shape in the early stage of milling, but changed to a spherical shape with the crystallite size about 30 nm after the milling. After sintering, the crystal structure of nanocrystalline NiAl intermetallic was assigned to B2 order NiAl phase with the average crystallite size about 100 nm. The nanocrystalline NiAl intermetallic exhibited prominent room temperature compressive properties, such as the true ultimate compressive strength and the fracture strain were 2143 MPa and 32.2%, respectively. The appearances of vein-like patterns on the fracture surface of NiAl intermetallic materials indicated that the fracture mechanism could be characterized as ductile fracture. It can be concluded that higher sintering density and nanocrystalline of NiAl intermetallic were benefited for the improvement of mechanical properties.     

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.     

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.     

Role of intensive milling in mechano-thermal processing of TiAl/Al2O3 nano-composite

In this research a nano-composite structure containing of an intermetallic matrix with dispersed Al₂O₃ particles was obtained via mechanical activation of TiO₂ and Al powder mixture and subsequent sintering. The mixture has been milled for different lengths of time and then as a subsequent process it has been sintered. Phase evolutions in the course of milling and subsequent sintering of the milled powder mixture were investigated. Samples were characterized by XRD, SEM, DTA and TEM techniques.The results reveal that the reaction begins during milling by formation of Al₂O₃ and L1₂ Al₃Ti and further milling causes partial amorphization of powder mixture. DTA results reveal that milling of the powder mixture causes solid state reaction between Al and TiO₂ rather than liquid–solid reaction. Also, it was observed that the exothermicity of aluminothermic reduction is reduced by increasing the milling time and the exothermic peak shifts to lower temperatures after partial amorphization of powder mixture during milling. Phase evolutions of the milled powders after being sintered reveal that by increasing the milling time and formation of L1₂ Al₃Ti in the milled powder, intermediate phase formed at 500 °C changes from D0₂₂ Al₃Ti to Al₂₄Ti₈ phase.     

Fabrication,mechanical properties and microstructure analysis of Si3N4/SiC nanocomposite

Ceramic nanocomposites, Si₃N₄ matrix reinforced with nano-sized SiC particles, were fabricated by hot pressing the mixture of Si₃N₄ and SiC fine powders with different sintering additives. Distinguishable increase in fracture strength at low and high temperatures was obtained by adding nano-sized SiC particles in Si₃N₄ with Al₂O₃ and/or Y₂O₃. Si₃N₄/SiC nanocomposite added with Al₂O₃ and Y₂O₃ demonstrated the maximum strength of 1.9 GPa with average strength of 1.7 GPa. Fracture strength of room temperature was retained up to 1400 as 1 GPa in the sample with addition of 30 nm SiC and 4 wt% Y₂O₃. Striking observation in this nanocomposite is that SiC particles at grain boundary are directly bonded to Si₃N₄ grain without glassy phases. Thus, significant improvement in high temperature strength in this nanocomposite can be attributed to inhibition of grain boundary sliding and cavity formation primarily by intergranular SiC particles, besides crystallization of grain boundary phase.     

Effects of ionic liquid additive [bmim]BF4 on fabrication of Ni-decorated Al2O3 powders by electroless deposition

Continuous and uniform Ni coating layer on the surface of Al₂O₃ powders are implemented by electroless deposition from sulfate solution with 25 g/L [bmim]BF₄ ionic liquid as additive. The effects of [bmim]BF₄ concentration on the surface morphologies, coating thickness, and element distribution of Ni-decorated Al₂O₃ powders have been investigated. It is demonstrated that with the increase of [bmim]BF₄ concentration in the range of 0–35 g/L, the formation of separated Ni powders and clusters away from Al₂O₃ surfaces are decreased. This can be explained by preferential adsorption of [bmim]BF₄ additive on the protrusions and sharp points of Al₂O₃ surface to inhibit the fast nucleation and crystal growth of Ni so that uniform Ni-decorated Al₂O₃ powders is obtained. When [bmim]BF₄ concentration is 25 g/L, the Ni grains on Al₂O₃ surface are uniform and spheroidal with a mean size of 0.5–1.5 μm and the coating thickness is about 2.0–3.0 μm. Besides, the deposition sequences of Ni coating layer is analyzed according to the changes in morphology of coated products obtained from different reaction stages. Furthermore, an empirical model of the deposition process of Ni-decorated Al₂O₃ powders with [bmim]BF₄ as additive is proposed to further elaborate the formation mechanism of the coating layer structure.     

The synthesis and characterization of ultrafine grain NiAl intermetallic

The nanocrystalline NiAl powders were synthesized by mechanical alloying (MA), and the ultrafine grain NiAl bulk materials were subsequently consolidated by vacuum hot-pressed sintering. The microstructure and mechanical properties of milled powders and bulk materials were characterized. The results reveal that the NiAl powders were synthesized after 1.67 h of milling and the grains of NiAl were refined to 18 nm after 22 h of milling. During milling, the temperature rise caused by MA led to the annealing effect and consequently resulted in the abnormal decrease in microstrain and microhardness. NiAl bulk material with a relative density of 99.4% was prepared after sintering at 1300 °C and its grain size was about 400 nm. Due to fine-grain strengthening, the compressive stress and compressive strain of NiAl bulk material were significantly improved at room temperature.     

Rapid consolidation of nanocrystalline 3Ni–Al2O3 composite from mechanically synthesized powders by high frequency induction heated sintering

Nanopowders of Ni and Al₂O₃ were synthesized from 3NiO and 2Al powders by high energy ball milling. Nanocrystalline Al₂O₃ reinforced composite was consolidated by high frequency induction heated sintering method within 2 min from mechanically synthesized powders of Al₂O₃ and 3Ni. The relative density of the composite was 96%. The average hardness and fracture toughness values obtained were 645 kg/mm² and 6.3 MPa m^1/2, respectively.     

Mechanical and magnetic properties of γ-Ni–xFe/Al2O3 composites

Ultra-fine grained γ-Ni–xFe (x = 20, 50, and 64 (nominal)) dispersed Al₂O₃-matrix composites were fabricated by a mechano-chemical process plus hot-pressing, and their mechanical and magnetic properties were explored. The results indicated that all composites incorporated with different γ-Ni–xFe alloys possessed high densities (relative density D ⩾ 98%) and sub-micrometer-sized matrix dispersed with γ-Ni–xFe particles of sizes below ∼500 nm. As compared to other two composite systems, γ-Ni–20Fe/Al₂O₃ had finer microstructures and displayed superior fracture toughness and strength. In high iron-contained γ-Ni–64Fe/Al₂O₃ composite undesired FeAl₂O₄ phase formed on the matrix grain boundaries, which is mainly responsible for its inferior mechanical properties. Although Young’s modulus and hardness of Ni–20Fe/Al₂O₃ composite system decreased, its fracture toughness increased monotonously with increasing the alloy content in the composition range investigated. Moreover, incorporation of ferromagnetic γ-Ni–xFe particles led all the composite systems to display ferromagnetism with their saturation magnetization increasing almost linearly with increasing alloy content. In addition, experiments showed that their ferromagnetism had high thermal stability (T_c = ∼580 °C), no obvious magnetism degradation and magnetic interactions of the alloys with the matrix being observed. The combination of good mechanical properties with excellent magnetic performance would make this material be very valuable in industry.     

Al3Ni2–Al composites with nanocrystalline intermetallic matrix produced by consolidation of milled powders

Mechanically alloyed nanocrystalline Al₆₃Ni₃₇ powder with a metastable structure of NiAl phase was mixed with 20, 30 and 40 vol.% of Al powder. The powder mixtures as well as pure powder of Al₆₃Ni₃₇ alloy were consolidated at 600 °C under the pressure of 7.7 GPa. The bulk materials were characterised by structural investigations (X-ray diffraction, light and scanning electron microscopy, energy dispersive spectroscopy), compression and hardness tests and measurements of density and open porosity. During the consolidation, the metastable NiAl phase transformed into the equilibrium Al₃Ni₂ intermetallic. The mean crystallite size of the Al₃Ni₂ intermetallic in the bulk materials is below 40 nm. The microstructure of the composite samples consists of Al₃Ni₂ intermetallic areas surrounded by lamellae-like Al regions. The hardness of the produced Al₃Ni₂–Al composites is in the range of 5–6.5 GPa (514–663 HV1), while that of the Al₃Ni₂ intermetallic is 9.18 GPa (936 HV1). The compressive strength of the composites increases with the decrease of Al content, ranging from 567 MPa to 876 MPa. The plastic elongation of the composites was increasing with the increase of Al content, while the Al₃Ni₂ intermetallic failed in the elastic region.     

Characterization and selection of optimal parameters to achieve the best tribological performance of the electrodeposited Cr nanocomposite coating

In this study, Nano particles were co-deposited with chromium from a hexavalent chromium bath by the conventional electrodeposition onto steel substrate as a cathode. The main goal of this work is to improve the wear and corrosion resistance, microhardness, coefficient of friction and select the best coating condition to satisfy these parameters using combined Analytic Hierarchy Process (AHP) – Technique for Order Preference by Similarity to Ideal Solution (TOPSIS) method. The dependence of the mentioned parameters was investigated in relation to the Al₂O₃, TiO₂, SiO₂ concentration in bath and particle size and it was found that the best tribological behavior improves by decreasing the particle size and increasing the particles concentration in the bath up to 10 g/l. AHP–TOPSIS method led to choose the Cr–Al₂O₃ nanocomposite coating achieved at 10 g/l Al₂O₃ content with mean particle size of 10 nm as the preferred alternative which is in good accordance with empirical findings.     

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 heat treatment on microstructure and adhesion of Al2O3 fiber-reinforced electroless Ni–P coating on Al–Si casting alloy

Influence of heat treatment regime on microstructure, phase composition and adhesion of Al₂O₃ fiber-reinforced Ni–P electroless coating on an Al–10Si–0.3 Mg casting alloy is investigated in this work. The pre-treated substrate was plated using a bath containing nickel hypophosphite, nickel lactate and lactic acid. Al₂O₃ fibers pretreated with demineralised water were placed into the plating bath. Resulting Ni–P–Al₂O₃ coating thickness was about 12 μm. The coated samples were heat treated at 400–550 °C/1–8 h. LM, SEM, EDS and XRD were used to investigate phase transformations. Adhesion of coating was estimated using scratch test with an initial load of 8.80 N. It is found that annealing at high temperatures (450 °C and above) leads to the formation of hard intermetallic products (namely Al₃Ni and Al₃Ni₂ phases) at the substrate–coating interface. However, as determined by the light microscopy and by the scratch test, these phases reduce the coating adhesion (compared to coatings treated by the optimal annealing regime 400 °C/1 h). The analysis of scratch tracks proves that fiber reinforcement significantly reduces the coating scaling. However, due to the formed intermetallic sub-layers, partial coating delamination may occur on the samples annealed at 450 °C and above.