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.     

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.     

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.     

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.     

Reaction mechanisms,resultant microstructures and tensile properties of Al-based composites fabricated in situ from Al-SiO2-Mg system

Reaction mechanisms, microstructures and tensile properties of the aluminum matrix composites made from Al-SiO₂-Mg system were investigated. When the temperature increased from room temperature to around 761 K, Mg dissolved into Al to form Mg-Al alloy. As the temperature increased to about 850 K, the remaining Mg reacted with SiO₂ to form MgO, Mg₂Si and Si as expressed in step reaction I: 6Mg + 2SiO₂ → 4MgO + Mg₂Si + Si. Finally, with a further increase in temperature, the remaining SiO₂ reacted with Al to produce Al₂O₃ and Si, while MgO reacted with Al₂O₃ to form MgAl₂O₄ as expressed in step reaction II: 4Al + 3SiO₂ + 2MgO → 2MgAl₂O₄ + 3Si. The Si also dissolved into matrix Al to form Al-Si alloy. Accordingly, its reaction process consisted of two steps and their apparent activation energies were 218 kJ/mol and 192 kJ/mol, respectively. As compared to the composites prepared by Al-SiO₂ system, its density increased from 2.4 to 2.6 g/cm³, and its tensile strength and elongation increased from 165 MPa and 3.95% to 187 MPa and 7.18%, respectively.     

Influence of yttrium dopant on the synthesis of ultrafine AlN powders by CRN route from a sol–gel low temperature combustion precursor

Y-doped ultrafine AlN powders were synthesized by a carbothermal reduction nitridation (CRN) route from precursors of Al₂O₃, C and Y₂O₃ prepared by a sol–gel low temperature combustion technology. The Y dopant reacted with alumina and thus forming yttrium aluminate of AlYO₃, Al₃Y₅O₁₂ and Al₂Y₄O₉, which formed a liquid at about 1400 °C and promoted the transformation of Al₂O₃ to AlN and the growth of AlN particles. Compared with the conventional solid CRN process, Y dopant reduced the synthesis temperature by 150 °C, and Al₂O₃ transformed to AlN completely at 1450 °C. The content of Y dopant had little effect on the synthesis temperature of AlN whereas it influenced the phase of Y compounds in the products. As the Y/Al molar ratio was in the range of 0.007648–0.022944, the particle sizes of Y-doped AlN powders synthesized at 1450 °C were 150–300 nm.     

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.     

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.     

Preparation of w–cu nano-composite powders with high copper content using a chemical co-deposition technique

A novel chemical co-precipitation was used to produce W-70%Cu nanocomposite powders with coating structure. The precursors consisting of CuC₂O₄·xH₂O and WO₃·2H₂O were first synthesized using copper nitrate, ammonium metatungstate(AMT) and oxalic acid as the raw materials at 80?°C for 1.5?h when the concentrations of the reactants were 0.8?mol/L and the hydrogen ion concentration was 1.2?mol/L. The precursors were calcined to produce the powders with different phase components and microstructure at various temperatures. The CuWO₄ and CuO nano-powders were obtained at 300?°C, which is colder than the traditional reaction temperature (1000?°C) of CuO?+?WO₃ = CuWO₄. However, the cubic Cu₂O and Cu₂WO₄ could be formed when the calcining temperature was 600?°C. The hydrogen reduction results show that the calcined powder is reduced to obtain W-Cu composite powder at 750?°C and 800?°C. In reduction process, volatile WO₂(OH)₂ through chemical vapor transport(CVT) continuously spreads to the copper surface and is reduced to form W and the coated particle is eventually formed. This particle is Cu particle coated by W phase and the interface between W and Cu phases is semi-coherent. It is found that the average particle size of the reduced powder is 30–50?nm observed by TEM images.     

Effect of aluminum source on the synthesis of AlN powders from combustion synthesis precursors

In the present work, the carbothermal reduction method was employed to fabricate the AlN powders by utilizing the combustion synthesized precursor derived from the mixed solution comprised of an aluminum source (Al(NO₃)₃ or Al₂(SO₄)₃ or AlCl₃), glucose, nitric acid, and urea. Effects of aluminum source on the particle size and morphology of precursors as well as synthesized AlN powders were studied in detail. The size and morphology of precursors, derived from various aluminum sources, had exhibited significant differences. The precursor from Al(NO₃)₃ source had completed the nitridation reaction at 1500 °C in 2 h. However, the nitridation reactions of the precursors from Al₂(SO₄)₃ or AlCl₃ source furnished at increased temperature of 1550 °C in 2 h. Moreover, the AlN powders from various aluminum sources have been synthesized directly from γ-Al₂O₃ without γ-Al₂O₃ to α-Al₂O₃ phase transition. The AlN powders from Al(NO₃)₃, calcined at 1550 °C for 2 h, were comprised of well-distributed spherical particles with an average size of 80 nm. While the AlN powders from AlCl₃ or Al₂(SO₄)₃ consisted of heterogeneously distributed spherical particles ranging from 100 to 200 nm or from 80 to 150 nm, respectively.     

SiC nanoparticle-reinforced Al2O3–Nb composite as a potential femoral head material in total hip arthroplasty

A ceramic–metal composite consisting of SiC nanoparticle-reinforced Al₂O₃ and Nb (referred to as SiC/Al₂O₃–Nb), was prepared and evaluated in vitro for potential application as a femoral head material in total hip arthroplasty. Dense bi-layer laminates of SiC nanoparticle-reinforced Al₂O₃ and Nb were fabricated by hot pressing of powders (1425 °C; 35 MPa), and evaluated using scanning electron microscopy, microchemical analysis, and mechanical testing. The flexural strength of the SiC/Al₂O₃–Nb laminate (960 ± 20 MPa) was higher than the value (720 ± 40 MPa) for an Al₂O₃–Nb laminate, and far higher than the value (620 ± 50 MPa) for SiC nanoparticle-reinforced Al₂O₃ (SiC/Al₂O₃). The Vickers hardness of SiC/Al₂O₃ was 17 ± 2 GPa, compared to 12 ± 1 GPa for Al₂O₃. A high interfacial shear strength of the SiC/Al₂O₃–Nb laminate (310 ± 100 MPa), coupled with SEM observation of the interfacial region, showed strong bonding between the SiC/Al₂O₃ and Nb layers. Composite femoral heads consisting of a SiC/Al₂O₃ surface layer and a Nb core could potentially lead to a reduction in the tendency for brittle failure as well as to lower wear, when compared to Al₂O₃ femoral heads.     

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.     

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.     

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.     

Limiting the development of Al4C3 to prevent degradation of Al/SiCp composites processed by pressureless infiltration

The presence of Al₄C₃ in Al/SiC composites may activate degradation of the material by its interaction with water; even moisture may cause its environmental degradation. It has been demonstrated that incorporation of 6 vol% SiO₂ powders into SiC_p preforms before processing by pressureless infiltration prevents formation of Al₄C₃. Analysis by electron back-scattered diffraction confirms that regardless of its crystal structure (α-quartz or α-cristobalite), SiO₂ completely reacts to form MgAl₂O₄. The metal/composite interface microstructure condition of the specimens processed under the most severe conditions (1100 °C for 60 min), four months later confirms the effectiveness of the SiO₂ powders.     

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.     

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.     

Joining of AlN and graphite disks using interlayer tapes by spark plasma sintering

AlN and graphite disks were successfully joined using a polymer plasticized ceramic tape as the interlayer by spark plasma sintering (SPS). The tape contains either composite powders of AlN and graphite or AlN powders without graphite. Both tapes contained 5 mass% Y₂O₃ as the sintering aid of AlN. The joining was carried out at 1700–1900 °C and 30 MPa for 5 min. No other reaction phase except for Al₂Y₄O₉ was identified in the joints. The maximum tensile strength of the joints was obtained when the AlN–graphite composite interlayer tape was used. The joining mechanism is attributed not to the chemical bonding, but to the physical bonding of the Al₂Y₄O₉ phase, which is solidified from the molten Al–Y–O squeezing into the porous graphite under pressure during SPS.     

Electrochemical fabrication of TiO2 nanoparticles/[BMIM]BF4 ionic liquid hybrid film electrode and its application in determination of p-acetaminophen

A water soluble ionic liquid, 1‐butyl‐3‐methylimidazolium tetrafluoroborate ([BMIM]BF₄), was incorporated into TiO₂ nanoparticles to fabricate a hybrid film modified glassy carbon electrode (nano‐TiO₂/[BMIM]BF₄/GCE) through electrochemical deposition in a tetrabutyltitanate sol solution containing [BMIM]BF₄. The obtained nano‐TiO₂/[BMIM]BF₄/GCEs were characterized scanning electronic microscopy (SEM) and X‐ray photoelectron spectroscopy (XPS). Electrochemical behaviors of p‐acetaminophen at the nano‐TiO₂/[BMIM]BF₄/GCEs were thoroughly investigated. Compared to the redox reaction of p‐acetaminophen using an unmodified electrode under the same conditions, a new reduction peak was observed clearly at 0.26 V with the modified electrode. In addition, the peak potential for the oxidation of p‐acetaminophen was found to shift negatively about 90 mV and the current response increased significantly. These changes indicate that the nano‐TiO₂/[BMIM]BF₄ hybrid film can improve the redox reactions of p‐acetaminophen in aqueous medium. Under optimum conditions, a linear relationship was obtained for the p‐acetaminophen solutions with concentration in the range from 5.0 × 10^? 8 to 5.0 × 10^? 5 M. The estimated detection limit was 1.0 × 10^? 8 M (S/N = 3). The newly developed method was applied for the determination of p-acetaminophen in urine samples.     

Mechanical properties of rolled A356 based composites reinforced by Cu-coated bimodal ceramic particles

Three kinds of A356 based composites reinforced with 3 wt.% Al₂O₃ (average particle size: 170 μm), 3 wt.% SiC (average particle size: 15 μm), and 3 wt.% of mixed Al₂O₃–SiC powders (a novel composite with equal weights of reinforcement) were fabricated in this study via a two-step approach. This first process step was semi-solid stir casting, which was followed by rolling as the second process step. Electroless deposition of a copper coating onto the reinforcement was used to improve the wettability of the ceramic particles by the molten A356 alloy. From microstructural characterization, it was found that coarse alumina particles were most effective as obstacles for grain growth during solidification. The rolling process broke the otherwise present fine silicon platelets, which were mostly present around the Al₂O₃ particles. The rolling process was also found to cause fracture of silicon particles, improve the distribution of fine SiC particles, and eliminate porosity remaining after the first casting process step. Examination of the mechanical properties of the obtained composites revealed that samples which contained a bimodal ceramic reinforecment of fine SiC and coarse Al₂O₃ particles had the highest strength and hardness.