Investigating effects of process parameters on microstructural and mechanical properties of Al5052/SiC metal matrix composite fabricated via friction stir processing

Friction stir processing (FSP) is a novel process for refinement of microstructure, improvement of material’s mechanical properties and production of surface layer composites. In this investigation via friction stir processing, metal matrix composite (MMC) was fabricated on surface of 5052 aluminum sheets by means of 5 μm and 50 nm SiC particles. Influence of tool rotational speed, traverse speed, number of FSP passes, shift of rotational direction between passes and particle size was studied on distribution of SiC particles in metal matrix, microstructure, microhardness and wear properties of specimens. Optimum of tool rotational and traverse speed for achieving desired powder dispersion in MMC was found. Results show that change of tool rotational direction between FSP passes, increase in number of passes and decrease of SiC particles size enhance hardness and wear properties.     

Characterization of oxide dispersion strengthened copper based materials developed by friction stir processing

The current study aims to show for the first time the ability of friction stir processing (FSP) in incorporating yttria particles into copper to produce an oxide dispersion strengthened material. The microstructure of the as-developed composites was characterized at various scales by light microscopy, electron probe microanalysis (EPMA) and scanning and transmission electron microscopy. The powder was found to be distributed in the Cu matrix as confirmed at various length scales from the micrometric to the nanometric level. The increase of the number of FSP passes leads to a more homogeneous and finer distribution of the particles as it favored the dissociation of the clusters of initial powder particles and the intergranular fracture of individual elemental particles. Transmission electron microscopy observations reveal that the constitutive crystallites of the initial powder, typically 10 nm in size, are frequently dissociated and dispersed into the copper matrix. In spite of their very low volume fraction, these 10 nm sized fragments which present the highest density among the various size classes of particles, exert a strengthening and work hardening effect.     

Microstructure and mechanical properties of hot extruded 6016 aluminum alloy/graphite composites

The incorporation of graphite particles into AA6016 aluminum alloy matrix to fabricate metal/ceramic composites is still a great challenge and various parameters should be considered. In this study, dense AA6016 aluminum alloy/(0-20 wt%) graphite composites have successfully been fabricated by powder metallurgy process. At first, the mixed aluminum and graphite powders were cold compacted at 200 MPa and then sintered at 500 ℃ for 1 h followed by hot extrusion at 450 ℃. The influence of ceramic phases(free graphite and in-situ formed carbides) on microstructure, physical and mechanical properties of the produced composites were finally investigated. The results show that the fabricated composites have a relative density of over 98%. SEM observations indicate that the graphite has a good dispersion in the alloy matrix even at high graphite content. Hardness of all the produced composites was higher than that of aluminum alloy matrix. No cracks were observed at strain less than 23% for all hot extruded materials.Compressive strength, reduction in height, ultimate tensile stress, fracture stress, yield stress, and fracture strain of all Al/graphite composites were determined by high precision second order equations. Both compressive and ultimate tensile strengths have been correlated to microstructure constituents with focusing on the in-situ formed ceramic phases, silicon carbide(SiC) and aluminum carbide(Al_4 C_3). The ductile fracture mode of the produced composites became less dominant with increasing free graphite content and in-situ formed carbides. Wear resistance of Al/graphite composites was increased with increasing graphite content. Aluminum/20 wt% graphite composite exhibited superior wear resistance over that of AA6016 aluminum alloy.     

Effect of surface functionalization on mechanical properties and decomposition kinetics of high performance polyetherimide/MWCNT nano composites

In this investigation, Polyetherimide (PEI) reinforced with multi-walled carbon nanotube (MWCNT) using novel melt blending technique. Surface of MWCNTs are modified by acid treatment as well as by plasma treatment. PEI nano composites with 2 wt% treated MWCNT shows about 15% improvement in mechanical properties when compared to unfilled PEI. The thermal decomposition kinetics of PEI/MWCNT nano composites has been critically analyzed by using Coats – Redfern model. The increase in activation energy for thermal degradation by 699 kJ/mol for 2 wt% MWCNT implies improvement in the thermal properties of PEI. Studies under Fourier Transform Infrared Spectroscopy (FTIR) and Transmission Electron Microscopy (TEM) depict significant interfacial adhesion with uniform dispersion of MWCNT in polymer matrix due to surface functionalization. 0.5 wt% chemically modified MWCNT shows typical alignment of MWCNT. There is a significant improvement in mechanical properties and thermal properties for surface functionalized MWCNT reinforced.     

Effects of copper addition on the in-situ synthesis of SiC particles in Al–Si–C–Cu system

In this research work, SiC particles have been successfully in-situ synthesized in Al–Si–Cu matrix alloy utilizing a novel liquid–solid reaction method. The effect of copper addition on the synthesis of SiC in Al–Si–C–Cu system was investigated. The composites mainly contain spherical SiC particles and θ-Al₂Cu eutectic phases, which are embedded in the α-Al matrix. Results indicated that the temperature for forming in-situ SiC particles significantly reduced from 750 °C to 700 °C with the copper addition. The size of in-situ synthesized SiC particles can be as low as 0.2 μm. Further study found that the addition of 10 wt.% copper into Al–Si–C alloy causes its solidus temperature to decrease by about 65 °C. Additionally, the Rockwell hardness value of SiCp/Al–18Si–5Cu composites has an average of 92, which is 50% higher than that of the sample without copper addition.     

Synthesis of spherical NiO nanoparticles through a novel biosurfactant mediated emulsion technique

Spherical nickel oxide nanoparticles were synthesized by microemulsion technique using rhamnolipids as the surfactant along with n-heptane and water. Nickel hydroxide (Ni(OH)₂) particles were first formed which were then calcined to obtain nickel oxide (NiO) particles. Scanning Electron Microscopy (SEM) studies revealed that the synthesized nickel hydroxide particles were spherical in shape with stacked lamellar sheets. Nickel hydroxide was converted to nickel oxide by calcinations at 600 °C for 3 h and was confirmed by X-ray Diffraction (XRD) analysis. Transmission Electron Microscopy (TEM) showed that the nickel oxide particles were crystalline and of uniform size. The effect of pH on particle size was investigated and it was found that the particle size decreased from 86 ± 8 nm at pH 11.6 to 47 ± 5 nm at pH 12.5. A novel method using rhamnolipid biosurfactant for microemulsion synthesis has been demonstrated which offers an eco-friendly alternative to conventional microemulsion technique based on organic surfactants.     

Effect of friction stir processing on erosion–corrosion behavior of nickel–aluminum bronze

In the present investigation, effects of Friction Stir Processing (FSP) on Erosion–Corrosion (E–C) behavior of Nickel–Aluminum Bronze (NAB) were studied by weight-loss measurements and surface characterization using an impingement jet test system. After FSP, the initial coarse microstructure of the cast NAB was transformed to a fine structure, and the porosity defects were eliminated. In addition, different FSP structures were produced by each rotation rate. Microhardness measurements showed a marked increase in FSP samples depending upon the FSP parameters. E–C tests were carried out by erodent at kinetic energies about 0.45 μJ and in 30°, 60° and 90° impact angles to simulate actual service conditions. The maximum weight-loss was observed in FSP samples and Scanning Electron Microscopy (SEM) results showed signs of brittle fracture mechanism in FSP samples. By gravimetric analysis, the degree of synergy was evaluated at 0.45 μJ kinetic energy at normal impact angle and negative synergy result implies the presence of a protective film on all sample surfaces.     

Processing, microstructure and mechanical properties of nickel particles embedded aluminium matrix composite

Nickel particles were embedded into an Al matrix by friction stir processing (FSP) to produce metal particle reinforced composite. FSP resulted in uniform dispersion of nickel particles with excellent interfacial bonding with the Al matrix and also lead to significant grain refinement of the matrix. The novelty of the process is that the composite was processed in one step without any pretreatment being given to the constituents and no harmful intermetallic formed. The novel feature of the composite is that it shows a three fold increase in the yield strength while appreciable amount of ductility is retained. The hardness also improved significantly. The fracture surface showed a ductile failure mode and also revealed the superior bonding between the particles and the matrix. Electron backscattered diffraction (EBSD) and transmission electron microscopy analysis revealed a dynamically recrystallized equiaxed microstructure. A gradual increase in misorientation from sub-grain to high-angle boundaries is observed from EBSD analysis pointing towards a continuous type dynamic recrystallization mechanism.     

Aluminium based composites strengthened with metallic amorphous phase or ceramic (Al2O3) particles

Two methods were used to obtain amorphous aluminium alloy powder: gas atomization and melt spinning. The sprayed powder contained only a small amount of the amorphous phase and therefore bulk composites were prepared by hot pressing of aluminium powder with the 10% addition of ball milled melt spun ribbons of the Al₈₄Ni₆V₅Zr₅ alloy (numbers indicate at.%). The properties were compared with those of a composite containing a 10% addition of Al₂O₃ ceramic particles. Additionally, a composite based on 2618A Al alloy was prepared with the addition of the Al₈₄Ni₆V₅Zr₅ powder from the ribbons used as the strengthening phase. X-ray studies confirmed the presence of the amorphous phase with a small amount of aluminium solid solution in the melt spun ribbons. Differential Scanning Calorimetry (DSC) studies showed the start of the crystallization process of the amorphous ribbons at 437 °C. The composite samples were obtained in the process of uniaxial hot pressing in a vacuum at 380 °C, below the crystallization temperature of the amorphous phase. A uniform distribution of both metallic and ceramic strengthening phases was observed in the composites. The hardness of all the prepared composites was comparable and amounted to approximately 50 HV for those with the Al matrix and 120 HV for the ones with the 2618A alloy matrix. The composites showed a higher yield stress than the hot pressed aluminium or 2618A alloy. Scanning Electron Microscopy (SEM) studies after compression tests revealed that the propagation of cracks in the composites strengthened with the amorphous phase shows a different character than these with ceramic particles. In the composite strengthened with the Al₂O₃ particles cracks have the tendency to propagate at the interfaces of Al/ceramic particles more often than at the amorphous/Al interfaces.     

Colloidal drug probe: Method development and validation for adhesion force measurement using Atomic Force Microscopy

This study demonstrates a novel technique of preparing drug colloid probes to determine the adhesion force between a model drug salbutamol sulphate (SS) and the surfaces of polymer microparticles to be used as carriers for the dispersion of drug particles from dry powder inhaler (DPI) formulations. Model silica probes of approximately 4 μm size, similar to a drug particle used in DPI formulations, were coated with a saturated SS solution with the aid of capillary forces acting between the silica probe and the drug solution. The developed method of ensuring a smooth and uniform layer of SS on the silica probe was validated using X-ray Photoelectron Spectroscopy (XPS) and Scanning Electron Microscopy (SEM). Using the same technique, silica microspheres pre-attached on the AFM cantilever were coated with SS. The adhesion forces between the silica probe and drug coated silica (drug probe) and polymer surfaces (hydrophilic and hydrophobic) were determined. Our experimental results showed that the technique for preparing the drug probe was robust and can be used to determine the adhesion force between hydrophilic/hydrophobic drug probe and carrier surfaces to gain a better understanding on drug carrier adhesion forces in DPI formulations.     

Fullerene/A5083 composites fabricated by material flow during friction stir processing

Fullerene was successfully dispersed into A5083 by friction stir processing (FSP). Dispersion of the fullerene enhanced the grain refinement by recrystallization during the FSP and the grain size reached ∼200 nm. The hardness was also remarkably increased by both the grain refinement and the dispersion of the fullerene molecules.In this study, material flow during the FSP was investigated with respect to the dispersion of the fullerene. It was revealed that the formation mechanism of the “onion ring” was closely related to the convectional flow induced by the shoulder of the rotating tool. This material flow by the shoulder is very important when fabricating the surface composites by the FSP in order to provide a uniform dispersion of the reinforcement.     

Fabrication of 5052Al/Al2O3 nanoceramic particle reinforced composite via friction stir processing route

In this research, microstructure and mechanical properties of 5052Al/Al₂O₃ surface composite fabricated by friction stir processing (FSP) and effect of different FSP pass on these properties were investigated. Two series of samples with and without powder were friction stir processed by one to four passes. Tensile test was used to evaluate mechanical properties of the composites and FSP zones. Also, microstructural observations were carried out using optical and scanning electron microscopes. Results showed that grain size of the stir zone decreased with increasing of FSP pass and the composite fabricated by four passes had submicron mean grain size. Also, increase in the FSP pass caused uniform distribution of Al₂O₃ particles in the matrix and fabrication of nano-composite after four passes with mean cluster size of 70 nm. Tensile test results indicated that tensile and yield strengths were higher and elongation was lower for composites fabricated by three and four passes in comparison to the friction stir processed materials produced without powder in the similar conditions and all FSP samples had higher elongation than base metal. In the best conditions, tensile strength and elongation of base material improved to 118% and 165% in composite fabricated by four passes respectively.     

Fatigue fracture of friction-stir processed Al–Al3Ti–MgO hybrid nanocomposites

This paper presents experimental results on the fatigue properties of Al-matrix nanocomposites prepared by the friction stir processing (FSP) technique. An Al–Mg alloy (AA5052) with different amounts (∼2 and 3.5 vol%) of pre-placed TiO₂ nanoparticles were FSPed up to 6 passes to attain homogenous dispersion of nano-metric inclusions. Microstructural studies by electron microscopic and electron back scattering diffraction (EBSD) techniques showed that nano-metric Al₃Ti (50 nm), TiO₂ (30 nm), and MgO (50 nm) particles were distributed throughout a fine-grained Al matrix (<2 μm). Consequently, a significant improvement in the tensile strength and hardness was attained. Uniaxial stress-controlled tension–tension fatigue testing (R = 0.1) were utilized to evaluate the fatigue behavior of the prepared nanocomposites. The results were compared with the un-processed (annealed) and FSPed alloy without pre-placing TiO₂ particles. It was found that FSP of the aluminum alloy increased the fatigue strength (at 10⁷ cycles) for about 28% and 32% compared with the annealed specimen when the concentration of the reinforcing particles was 2 and 3.5 vol%, respectively. Fractographic analysis determined a ductile fracture behavior with deep-equiaxed dimples for the annealed and FSPed alloy. The facture surface of the nanocomposites revealed a combined ductile–brittle fracture mode with finer dimples. The mechanism of the fatigue fracture and the role of nano-metric inclusions were elaborated.     

Carbon-nanofibre-reinforced poly(ether ether ketone) composites

Poly(ether ether ketone) nanocomposites containing vapour-grown carbon nanofibres (CNF) were produced using standard polymer processing techniques. Evaluation of the mechanical composite properties revealed a linear increase in tensile stiffness and strength with nanofibre loading fractions up to 15 wt% while matrix ductility was maintained up to 10 wt%. Electron microscopy confirmed the homogeneous dispersion and alignment of nanofibres. An interpretation of the composite performance by short-fibre theory resulted in rather low intrinsic stiffness properties of the vapour-grown CNF. Differential scanning calorimetry showed that an interaction between matrix and the nanoscale filler could occur during processing. Such changes in polymer morphology due to the presence of a nanoscale filler need to be considered when evaluating the mechanical properties of such nanocomposites.     

The measurement of the adhesion force between ceramic particles and metal matrix in ceramic reinforced-metal matrix composites

This paper presents the method for measurement of the adhesion force and fracture strength of the interface between ceramic particles and metal matrix in ceramic reinforced-metal matrix composites. Three samples with the following Cu to Al₂O₃ ratio (in vol.%) were prepared: 98.0Cu/2.0Al₂O₃, 95.0Cu/5.0Al₂O₃ and 90Cu/10Al₂O₃. Furthermore, microwires which contain a few ceramic particles were produced by means of electro etching. The microwires with clearly exposed interface were tested with use of the microtensile tester. The microwires usually break exactly at the interface between the metal matrix and ceramic particle. The force and the interface area were carefully measured and then the fracture strength of the interface was determined. The strength of the interface between ceramic particle and metal matrix was equal to 59 ± 8 MPa and 59 ± 11 MPa in the case of 2% and 5% Al₂O₃ to Cu ratio, respectively. On the other hand, it was significantly lower (38 ± 5 MPa) for the wires made of composite with 10% Al₂O₃.     

Preparation of TiN–Ti5Si3 in-situ composites by Selective Laser Melting

The Selective Laser Melting (SLM) Rapid Manufacturing (RM) of the high-energy ball milled Ti–Si₃N₄ composite powder with the mol ratio of 9:1 was performed in the present work. The microstructural characterizations revealed the formation of TiN reinforced Ti₅Si₃ matrix composites after laser processing via the in-situ synthesis reaction 9Ti + Si₃N₄ = 4TiN + Ti₅Si₃. The in-situ presented TiN reinforcing phase possessed a refined granular morphology and a uniform distribution throughout the Ti₅Si₃ matrix, showing a clear and compatible interfacial structure with the matrix. The metallurgical mechanisms for the in-situ synthesis of TiN reinforced Ti₅Si₃ matrix composites by SLM were also proposed.     

Dispersion and roles of montmorillonite on structural,flammability, thermal and mechanical behaviours of electron beam irradiated flame retarded nanocomposite

In this work, the effects of montmorillonite (MMT) dispersion and electron beam irradiation on intercalation and flammability-thermal behaviours of alumina trihydrate (ATH) added low density polyethylene and ethylene vinyl acetate (LDPE–EVA) blends were investigated. MMT and ATH added LDPE–EVA blends were compounded using Brabender mixer and compression moulded into sheets. The samples sheets were electron beam irradiated in the dosage range of 0 to 250 kGy. The dispersion and intercalation of nano-MMT in LDPE–EVA matrix were investigated through X-ray diffraction (XRD) analysis. The d-spacing measurements revealed that the addition of nano-MMT has effectively intercalated into polymer matrix and this has enhanced the compatibility of ATH particles and LDPE–EVA matrix. Limiting oxygen index test (LOI) revealed that the incorporation of MMT into ATH added LDPE–EVA blends as improved the flame retardancy up to 26.5 LOI%. Besides, the application of electron beam irradiation were also improved the flame retardancy of the blends by increasing the LOI% for about 2% compared to non-irradiated samples. The application of irradiation dosage up to 250 kGy has rapidly improved the thermal stability of blends by delaying decomposition temperature and also promoting formation of char. The increasing of MMT loading level and irradiation dosage has effectively enhanced tensile strength and Young’s modulus by intercalating polymer matrix into interlayer galleries of MMT particles. Beside, the formation of crosslinking networks in polymer matrix also could further enhance the tensile strength and Young’s modulus. The intercalation effect of MMT particles and formation of crosslinking networks in polymer matrix could improve the thermal and mechanical properties. Consequently, this study has demonstrated that addition of MMT and electron beam irradiation into ATH added LDPE–EVA blends could produce better flammability, thermal and physical properties of ATH added LDPE–EVA blends.     

Microstructure characteristics and mechanical properties of cold metal transfer welding Mg/Al dissimilar metals

AZ31B Mg alloy and 6061 Al alloy were joined by using cold metal transfer (CMT) welding with pure copper (HS201) as the filler metal. The microstructure of Mg/Al CMT weld joint was studied by means of Optical Microscopy, Scanning Electron Microscope (SEM), Energy Dispersive X-ray (EDX), X-ray Diffraction (XRD). Results showed that dissimilar metals of Mg/Al could be successfully joined by CMT under proper processing parameters. The bonding strength of the joint was 34.7 MPa. A variety of Al–Cu intermetallic compounds, i.e. AlCu, CuAl₂, Cu₉Al₄, presented in the fusion zone of Al side, and Cu based solid solution was generated in weld zone, while Cu₂Mg and Al–Cu–Mg ternary eutectic structure was formed in the fusion zone of Mg side. The micro-hardness in the both sides of fusion zones increased sharply, which were 362 HV in Mg side and 260 HV in Al side. The joint was brittle fractured in the intermetallic compound layer of the fusion zone of Mg side, where plenty of Cu₂Mg intermetallic compounds were distributed continuously.     

Increase of bending fatigue resistance for tungsten inert gas welded SS400 steel plates using friction stir processing

To improve the fatigue resistance of tungsten inert gas (TIG)-welded SS400 steel plates, friction stir processing (FSP) was performed on TIG weld beads. Although the tensile properties of the TIG-welded steel plates with FSP were similar to those without FSP, their bending strength exhibited about 1.4 GPa at room temperature, which was 40% higher than that without FSP (about 1 GPa). Similarly, FSP produced about 170% increase in the number of cycles to failure at an applied stress amplitude of 270 MPa during three-point bending fatigue at room temperature. A fine-grained FSP region (grain sizes of about 1–2 μm in diameter) enhanced grain-boundary strengthening, leading to the higher bending strength and bending fatigue resistance.     

(Cu,Fe, Co,or Ni)-doped tin dioxide films deposited by spray pyrolysis: Doping influence on thermal stability of the film structure

The results of doping influence on thermal stability of the SnO₂ film morphology are presented in this article. The SnO₂ films doped by Fe, Cu, Ni, Co (16 at.%) were deposited by spray pyrolysis from 0.2 M SnCl₄–water solution at T_pyr 350–450 °C. The annealing at 850–1030 °C was carried out in the atmosphere of the air. The change of such parameters as film morphology, the grain size, texture and the intensity of X-ray diffraction (XRD) peaks have been controlled. For structural analysis of tested films we have been using X-ray diffraction, Scanning Electron Microscopy (SEM), and Atomic Force Microscopy (AFM) techniques. It was established that the doping does not improve thermal stability of both film morphology and the grain size. It was made a conclusion that the increased contents of the fine dispersion phase of tin oxide in the doped metal oxide films, and the coalescence of this phase during thermal treatment are the main factors, responsible for observed changes in the morphology of the doped SnO₂ films.