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.     

Synthesis and characterisation of nanostructured Al–Al3V and Al–(Al3V–Al2O3) composites by powder metallurgy

In this study, the formation and characterisation of Aluminium (Al)-based composites by mechanical alloying and hot extrusion were investigated. Initially, the vanadium trialuminide (Al₃V) particles with nanosized structure were successfully produced by mechanical alloying and heat treatment. Al₃V–Al₂O₃ reinforcement was synthesised by mechanochemical reduction during milling of V₂O₅ and Al powder mixture. In order to produce composite powders, reinforcement powders were added to pure Al powders and milled for 5?h. The composite powders were consolidated in an extrusion process. The results showed that nanostructured Al-10?wt-% Al₃V and Al-10?wt-% (Al₃V–Al₂O₃) composites have tensile strengths of 209 and 226?MPa, respectively, at room temperature. In addition, mechanical properties did not drop drastically at temperatures of up to 300°C.     

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.     

Fabrication of nano-sized Al2O3 reinforced casting aluminum composite focusing on preparation process of reinforcement powders and evaluation of its properties

In this study, a novel approach was used to fabricate Al₂O₃ nanoparticle reinforced aluminum composites to avoid agglomeration of nanoparticles in matrix. Al₂O₃ nanoparticles were separately milled with aluminum and copper powders at different milling durations and incorporated into A356 alloy via stir casting method. The effects of milling process and milling time on mechanical properties of the composites were evaluated by hardness, tensile, and compression tests. Based on the results, some of the composites, reinforced with Al₂O₃-metallic mixed powders, showed higher mechanical performance compared with that of the pure Al₂O₃ nanoparticle reinforced composite. This enhancement is related to uniform distribution of individual nanoparticles and grain refinement of A356 matrix, shown in microstructural studies. Moreover, the results showed that an increase in milling time, led to a gradual decrease in mechanical performance of the samples. It can be related to further oxidation of metallic powders that can act as inclusions and also further probable contamination of nanoparticles with increase in milling time. Studies on the fracture surfaces revealed that the failure of matrix was the basic mechanism of fracture in the composites. Agglomerated nanoparticles were observed on dendrites in the fracture surface of the Al₂O₃–Al reinforcement samples.     

Effect of mechanical milling on the corrosion behavior of Al–Zn/Al<Subscript>2</Subscript>O<Subscript>3</Subscript> composite in NaCl solution

Ceramic particle reinforced aluminum metal matrix composites (MMCs) have resulted in potential use in aerospace and automobile industries. The composites have been processed by mechanical milling followed by traditional powder metallurgy route. The Al crystallite size is reduced to 27 nm after 60 h of milling. Results of the corrosion tests, evaluated using the potentiodynamic method in the NaCl solution, indicate that corrosion of the investigated composite materials depends on the weight fraction of the reinforcing particles. It has been found out, based on the determined anode polarization curves, that the investigated materials are susceptible to pitting corrosion. Moreover, experimental results suggest that the milled composite material Al–Zn/Al₂O_3p has higher corrosion resistance in the selected environment compared to unmilled composite Al–Zn/Al₂O_3p. Polarization curves show that the milling procedure improves the composite corrosion resistance in passive conditions. This is illustrated by the corrosion potential, which becomes nobler with milling.     

Tribological properties of Al6061–Al2O3 nanocomposite prepared by milling and hot pressing

Tribological properties of bulk Al6061–Al₂O₃ nanocomposite prepared by mechanical milling and hot pressing were investigated. Al6061 chips were milled for 30 h to achieve a homogenous nanostructured powder. A 3 vol.% Al₂O₃ nanoparticles (∼30 nm) were added to the Al6061 after 15 and 30 h from the beginning of milling. The milling times with Al₂O₃ in these two samples were then 15 h and 30 min, respectively. Additionally, 3 vol.% Al₂O₃ (1 μm and 60 μm) was added to the Al6061 after 15 h of milling; where, the micron size Al₂O₃ in these two samples, was milled 15 h with the matrix. Hot pressing of milled samples was executed at 400 °C under 128 MPa pressure in a uniaxial die. The hot pressed samples were characterized by micro-hardness test, bulk density measurements, pin on disc wear test, and finally scanning electron microscopy observations. Fifteen hour-milled nanocomposite with nanoscale Al₂O₃, showed improvement in wear resistance and bulk density compared with that of 30 min-milled nanocomposites due to better dispersion of Al₂O₃ nanoparticles, improved surface quality of nanocomposite particles before pressing and more grain refinement of Al matrix. Moreover, increasing the reinforcement size increased the wear rate because of reduction in relative density, hardness and inter-particle spacing.     

Fabrication and characterisation of copper–alumina nanocomposites prepared by high-energy fast milling

Two different methods are used to prepare Cu–20 vol-% Al₂O₃ nanocomposite powders via high-energy planetary fast milling. In the solid solution method, CuO powder was added to the Cu–Al solid solution powder, and the composite was fabricated by milling after 100?h. In the direct mixing method, Cu and Al₂O₃ powders were mechanically milled via high-energy planetary fast milling for 100?h. The transition electron micrographs (dark and white fields) revealed the presence of Al₂O₃ nanoparticles in crystalline Cu matrices for both methods. However, the density and bending strength of the nanocomposites produced via the solid solution method were higher than those of the samples produced via the direct mixing method.     

Chemical stability of carbon nanotubes in the 2024Al matrix

Five volume percent of carbon nanotubes and 2024Al alloy powder were mixed with ball milling method, and then the composite was fabricated at 873 K by hot pressing sintering technique. The microstructure of the composite was investigated using optical microscopy, transmission electron microscopy, and X-ray diffraction. The experimental results showed that carbon nanotubes are reacted and changed into Al₄C₃. Nano-Al₄C₃ phases with needle shape are distributed mainly on Al grain boundaries; meanwhile some of them exist within Al grains. The reaction mechanism of carbon nanotubes-Al is discussed.     

Formation and sintering of 75 mol% alumina/25 mol% zirconia (2–3.5 mol% yttria) composite powder prepared by the hydrazine method

Al₂O₃/Y₂O₃-doped ZrO₂ composite powders with 25 mol% ZrO₂ have been prepared by the hydrazine method. As-prepared powders are the mixtures of AlO (OH) gel solid solutions and amorphous ZrO₂. The formation process leading to -Al₂O₃/t-ZrO₂ composite powders is investigated. Hot isostatic pressing has been performed for 1 h at 1500 °C under 196 MPa. Dense ZrO₂-toughened Al₂O₃ (ZTA) ceramics with homogeneous-dispersed ZrO₂ particles show excellent mechanical properties. The toughening mechanism is discussed.     

NiAl-Al2O3 intermetallic matrix composite prepared by reactive milling and consolidation of powders

Reactive milling of nickel oxide and aluminium powders corresponding to the stoichiometric reaction 3NiO + 5Al resulted in the formation of intermetallic matrix composite NiAl-Al₂O₃, with 28 wt% of alumina. Prolongation of the milling process allowed obtaining the microstructure with nanosize range of crystallites of both phases, as showed XRD measurements and TEM observations. The refinement of microstructure was accompanied with an increase of lattice strain as a result of ball milling. The particles size and morphology changed from several tens of micrometers and polyhedron shape observed immediately after the reaction took place, to several micrometers and spherulitic shape after long-term milling. Two consolidation techniques of nanocomposite powders were applied: explosive compaction and hot-pressing under high pressure. Both methods allowed obtaining the samples of high density (up to 99% of theoretical one) and microhardness above 13 GPa. Simultaneously, a nanocrystalline structure of the material was preserved.     

Synthesis of LaB<Subscript>6</Subscript>–Al<Subscript>2</Subscript>O<Subscript>3</Subscript> nanocomposite powders via ball milling-assisted annealing

In this study, LaB₆–Al₂O₃ nanocomposite powders were synthesized via ball milling-assisted annealing process starting from La₂O₃–B₂O₃–Al powder blends. High-energy ball milling was conducted at various durations (0, 3, 6 and 9 h). Then, the milled powders were annealed at 1200 °C for 3 h under Ar atmosphere in order to obtain LaB₆ and Al₂O₃ phases as reaction products. X-ray diffractometry (XRD), scanning electron microscopy/energy-dispersive spectrometry (SEM/EDS) and transmission electron microscopy (TEM) techniques were utilized to carry out microstructural characterization of the powders. No reaction between the reactants was observed in the XRD patterns of the milled powders, indicating that high-energy ball milling did not trigger any chemical reactions even after milling for 9 h. LaAlO₃ and LaBO₃ phases existed in the annealed powders which were milled for 0, 3 and 6 h. LaBO₃ phase was removed after HCl leaching. 9-h milled and annealed powders did not exhibit any undesired phases such as LaAlO₃ and LaBO₃ after leaching step, and pure nanocrystalline LaB₆–Al₂O₃ composite powders were successfully obtained. TEM analyses revealed that very fine LaB₆ particles (~?100 nm) were embedded in coarse Al₂O₃ (~?500 nm) particles.     

Effect of high energy ball milling on the displacement reaction in particulate reinforced Al–Si–Cu alloy matrix composite powders

The displacement reaction between Al and SiO₂ in an Al–3wt%Cu–3wt%Si–9wt%SiO₂ powder mixture has been studied when the mixture had been ball-milled, and compared with the reaction in the as-mixed powder. Diffusion couples consisting of Al/SiO₂ were formed during ball milling. The size of the composite powder particles and the diffusion couples was reduced by increasing the ball milling time. Differential thermal analysis and X-ray diffraction results showed that the displacement reaction between Al and SiO₂ did not occur in the as-mixed powder, but occurred in the as-milled powders in the temperature range of 640–680 °C. Furthermore, the onset temperature of the displacement reaction shifted to lower temperatures after increasing the ball milling time. On the basis of these results the milled powder was sintered at 640 °C in order to produce an Al–Cu–Si matrix composite reinforced with homogeneously distributed submicron-sized Al₂O₃ particles. This is much lower than the temperature required for the same reaction in other processes which are used to produce such composites, such as the melting infiltration process.     

Pulvermetallurgische Erzeugung von SiC‐ und Al2O3‐verstärkten Al‐Cu‐Legierungen

Powder metallurgical fabrication of SiC and Al₂O₃ reinforced Al‐Cu alloys Based on metallographic studies the states of composite powder formation during high‐energy ball milling will be discussed. Spherical powder of aluminium alloy AA2017 was used as feedstock material for the matrix. SiC and Al₂O₃ powders of submicron and micron grain size (<2 μm) were chosen as reinforcement particles with contents of 5 and 15 vol.‐% respectively. The milling duration amounted to a maximum of 4 hours. The abrasion of the surface of the steel balls, the rotor and the vessel is indicated by the content of ferrous particles in the powder. High‐energy ball milling leads to satisfying particle dispersion for both types of reinforcement particles. Further improvements are intended. The microstructure of compact material obtained by hot isostatic pressing and extrusion was studied in detail by scanning and transmission electron microscopy. For both types of reinforcement the microstructure of composites is similar. The microporosity is low. The interface between reinforcement particles and matrix is free of brittle phases and microcracks. In the case of SiC reinforcement particles, a small interface interaction is detectable which implies a good embedding of reinforcement particles. High‐energy ball milling under air‐atmosphere leads to the formation of the spinel phase MgAl₂O₄ during the subsequent powder‐metallurgical processing. Because of the size, rate and dispersion of the spinel particles, an additional reinforcement effect is expected.     

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.     

Effects of ball milling and high-pressure torsion for improving mechanical properties of Al–Al2O3 nanocomposites

Pure Al powders were mixed with a 30 % volume fraction of Al₂O₃ powders having particle sizes of ~30 nm. The mixed powders were first subjected to ball milling (BM) and thereafter consolidated by high-pressure torsion (HPT) at room temperature under a pressure of 3 GPa for 10 turns. The Al–Al₂O₃ composite produced by BM and HPT (BM + HPT) had a more uniform dispersion of the nano-sized Al₂O₃ particles in the Al matrix. Hardness values of the BM + HPT composites were higher than those of the composites without BM. It is shown that the use of BM powders for HPT is more effective in achieving a uniform dispersion of the nano-sized Al₂O₃ particles and in improving mechanical properties of the Al–Al₂O₃ nanocomposites.     

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.     

Quasicrystalline phase formation during heat treatment in mechanically alloyed Al65Cu20Fe15 alloy

Abstract

Quasicrystalline phase formation during heat treatment in the mechanically alloyed Al₆₅Cu₂₀Fe₁₅ powders was studied by X-ray diffraction (XRD) and differential scanning calorimeter (DSC). The mechanical alloying was performed at speed of 300 rev min^–1 for times up to 70 h. It was found that mechanical alloying of the Al₆₅Cu₂₀Fe₁₅ powders did not result in the quasicrystalline (QC) icosahedral phase (i-phase) formation. The long time milling resulted in the formation of a cubic Al (Cu,Fe) solid solution phase (β-phase). The cubic Al (Cu,Fe) solid solution identified as β-phase was observed to be present as one of the major phases in the Al₆₅Cu₂₀Fe₁₅ alloy. The formation of the quasicrystalline icosahedral phase (i-phase) was only observed for short time milled powders after additional annealing at temperature above 500°C. The present investigation also showed that a tetragonal Al₂Cu phase (θ-phase) forms with short time milling. The tetragonal Al₇Cu₂Fe₁ phase (w-phase) was observed after heat treatment of the short time milled and unmilled powders. The present investigation indicated that an effective process to prepare the quasicrystalline materials was using a combination of short time milling and subsequent annealing.     

Interaction between liquid aluminum and NiO single crystals

The wetting behavior of NiO single crystal by liquid aluminum has been studied by the sessile drop method under vacuum at 973–1273 K for 2 h. Optical microscopy, SEM, EDS and X-ray analysis were applied to characterize the structure and chemistry of solidified cross-sectioned sessile drop couples. Under tested conditions, molten Al wets and reacts with NiO to form Al₂O₃ and Ni. This leads to alloying of the initially pure Al drop with Ni to the hypereutectic composition and to the formation of a thick reaction product region inside the NiO substrate, whose structure presents interpenetrated networks of fine alumina precipitates and an Al–Ni matrix. After solidification the Al–Ni matrix and the drop have the same phase composition, which is in agreement with Al–Ni phase diagram, showing the formation of Al₃Ni at T < 1128 K and Al₃Ni₂ at 1128 K < T < 1406 K. The strong reactivity of Al/NiO couples, accompanied with the drop deformation, fragmentation of the reaction product region and development of a crater under the drop, contributes to the perturbation of the triple line and to the formation of apparent contact angles at 1073–1273 K. This leads to unusual changes of measured contact angles with temperature, decreasing from 84^° at 973 K to 36^° at 1073 K, and then increasing to 75^° at 1273 K, while structural analysis suggests complete wetting at 1073 K.     

A technique for the fabrication of fully dense Ca-rich plagioclase (An70-An100) samples suitable for studying the plastic rheology of bytownite (An80)

Two different types of solid samples of bytownite (Ca_0.7Na_0.3Al₂Si₂O₈ to Ca_0.9Na_0.1Al₂Si₂O₈) composition were fabricated from synthetic crystal and glass powders. The crystal and the glass powders were produced by crystallisation or melting of a gel of bytownite composition. Cold pressing under vacuum followed by hot isostatic pressing (hip) of the powders produced fully dense samples composed either of 100% bytownite crystals or of 90% bytownite crystals and 10% bytownite glass. The cold-pressed samples were composed of a matrix of nanometer sized bytownite needles and larger crystals of up to 3 m in size. During hot pressing the grain sizes in the matrix increased slightly while larger crystals increased to close to 4 m. The rheological behaviour of the hot isostaticly pressed samples for cases of tri axial compression and torsion was tested in a gas confining deformation apparatus at high temperature and confining pressure. Grain growth was observed during the deformation experiments. The maximum flow stress was typically less than 200 MPa and was attained by sample strain of 10% during axial compression and a shear strain of 1.0 during torsion. The resulting microstructures were dominated by fibrous grains for the compressive deformation and by more round-shaped grain boundaries during torsion. Both type of experiments induced a preferred shape and crystallographic orientation.     

Effect of Ni addition on formation of amorphous and nanocrystalline phase during mechanical alloying of Al-25 at.%Fe-(5,10) at.%Ni powders

Al-Fe-Ni ternary powder mixtures containing 25 at.%Fe-5 at.%Ni and 25 at.%Fe-10 at.%Ni were mechanically alloyed by a high-energy planetary ball mill. Structural evolution of these powders during milling was investigated by X-ray diffraction technique and transmission electron microscopy. Almost complete amorphous phase in Al₇₀Fe₂₅Ni₅ system is observed at the early milling stage. The amorphous phase transforms into metallic compound Al₅(Fe,Ni)₂ and then the compound changes to ordered Al(Fe,Ni) phase. The last milling products in Al₇₀Fe₂₅Ni₅ system are amorphous phase plus nanocrystalline of the disordered Al(Fe,Ni) phase changed from the ordered Al(Fe,Ni) phase. During milling of Al₆₅Fe₂₅Ni₁₀ system, α-Al and α-Fe solid solutions formed at the early stage change to the ordered Al(Fe,Ni) compound and at last the ordered phase changes to the disordered Al(Fe,Ni) phase. Ten percent of Ni addition promotes retardation of the formation of the amorphous phase.