Microstructures and mechanical properties of spark plasma sintered Cu–Cr composites prepared by mechanical milling and alloying

Nanograined Cu–8 at.% Cr composite was produced by a combination of mechanical milling (MM), mechanical alloying (MA) and spark plasma sintering (SPS). Commercial Cu and Cr powders were pre-milled separately by MM. The milled Cu and Cr powders were then mechanically alloyed with as-received Cr and Cu powders respectively. After milling, the powder mixtures were separately subjected to SPS. It was found that pre-milling Cr can efficiently decrease the size of grain and reinforcement, resulting in remarkable strengthening. The grain size of Cu matrix was about 82 nm after SPS. The Vickers hardness, compressive yield strength and compression ratio of the composite were 327 HV, 1049 MPa and 10.4%, respectively. The excellent mechanical properties were primarily attributed to dispersion strengthening of the Cr particles and fine grain strengthening of the Cu matrix. The strong Cu/Cr interface and dissolved Cr atoms can also contribute to strengthening of the composite.     

Structural and microstructural characterizations of nanocrystalline hydroxyapatite synthesized by mechanical alloying

Single phase nanocrystalline hydroxyapatite (HAp) powder has been synthesized by mechanical alloying the stoichiometric mixture of CaCO₃ and CaHPO₄ powders in open air at room temperature, for the first time, within 2 h of milling. Nanocrystalline hexagonal single crystals are obtained by sintering of 2 h milled sample at 500 °C. Structural and microstructural properties of as-milled and sintered powders are revealed from both the X-ray line profile analysis and transmission electron microscopy. Shape and lattice strain of nanocrystalline HAp particles are found to be anisotropic in nature. Particle size of HAp powder remains almost invariant up to 10 h of milling and there is no significant growth of nanocrystalline HAp particles after sintering at 500 °C for 3 h. Changes in lattice volume and some primary bond lengths of as-milled and sintered are critically measured, which indicate that lattice imperfections introduced into the HAp lattice during ball milling have been reduced partially after sintering the powder at elevated temperatures. We could achieve ~ 96.7% of theoretical density of HAp within 3 h by sintering the pellet of nanocrystalline powder at a lower temperature of 1000 °C. Vickers microhardness (VHN) of the uni-axially pressed (6.86 MPa) pellet of nanocrystalline HAp is 4.5 GPa at 100 gm load which is close to the VHN of bulk HAp sintered at higher temperature. The strain-hardening index (n) of the sintered pellet is found to be > 2, indicating a further increase in microhardness value at higher load.     

The Cu matrix cermets remarkably strengthened by TiB2 “in situ” synthesized via self-propagating high temperature synthesis

The TiB₂–Cu cermets with predominant concentration of superhard TiB₂ (from 45 to 90 vol.%) were fabricated using elemental powders by means of SHS (self-propagating high-temperature synthesis) process and simultaneously densified by p-HIP (pseudo-isostatic pressing technique). The heat released during highly exothermic SHS reaction was “in situ” utilized for sintering. The combustion occurred even for 50 vol.% Cu dilution. According to XRD metallic copper binder was formed in those cermets in whole range of investigated compositions. The TiB₂ volume fraction significantly influenced the properties of fabricated materials, especially grain size and hardness. Both the average grain size and hardness significantly increased with TiB₂ content, so the maximum value of 18 GPa was measured for TiB₂–5 vol.%Cu composite. Coarse grains of 6.4 μm in size were observed for this composite while TiB₂-based submicro-composites were formed for 40–50% of Cu where the average grain size did not exceed 0.6 μm. The Vickers hardness of 16–18 GPa obtained for cermets containing from 85 to 90 vol.% of TiB₂ and no radial cracks in Vickers hardness test proved that in term of hardness and fracture toughness the composites might be competitive to WC–Co cermets.     

Effect of milling speed and shaping method on mechanical properties of nanostructure bulked aluminum

Nanostructured bulk Al was successfully fabricated by conventional powder metallurgy, hot press and extrusion. Effect of milling speed on mechanical properties was investigated. Morphology of milled powders was monitored by scanning electron microscope (SEM). The relative density and hardness were measured by Archimedes and Vickers methods, respectively. Tensile and compression experiments were used for the measurement of mechanical properties. Results showed that a nanostructured Al powder was obtained after ball milling. Maximum relative density and hardness were procured for hot press (HP) samples at 360 rpm milling speed. There is a considerable improvement in yielding point (YP) at higher milling speed in both HP and extrude (EX) methods. Maximum YP of 315 MPa was obtained for EX samples that are larger than YP in HP samples (243 MPa).     

Intergranular alumina–SiC micro-nanocomposites sintered by spark plasma sintering

Alumina–5 vol% SiC micro-nanocomposites with almost completely intergranular microstructure were produced by spark plasma sintering (SPS). Before sintering, well dispersed slurries were obtained by ball-milling of powders using an electrosteric dispersant in aqueous media. High density composites could be achieved at lower sintering temperatures by SPS, as compared with hot pressing (HP) sintering process. Microstructure studies show that the nano-SiC particles were mainly located at the alumina grain boundaries.     

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.     

The thermal stability of high-energy ball-milled nanostructured Cu

The thermal stability of nanostructured (NS) Cu prepared by high-energy ball milling was investigated. The as-prepared samples were isothermal annealed for 1 h in the temperature range of 200–1000 °C. Effects of annealing on NS Cu samples were studied by means of Vickers hardness test, differential scanning calorimetry (DSC) and stress relaxation test. The exceptional high microhardness of as-prepared Cu sample of 1.7 GPa was not detected to decrease after annealing at 500 °C for 1 h with corresponding small value of activation volumes V^* of 22.6b³ and high value of strain rate sensitivity m of 0.0176. A prominent decrease of microhardness was detected after higher temperature annealing with a rapidly increase of activation volume and decrease of strain rate sensitivity. The present investigation demonstrates that the thermal stability of NS Cu prepared by high-energy ball milling is determined by not only the grain size but also the microstructure of grain boundaries, and during annealing process, the strain release process occurred prior to the grain growth process, therefore, the NS Cu has a relatively high thermal stability.     

Mechanical properties of nanostructured Al2024–MWCNT composite prepared by optimized mechanical milling and hot pressing methods

Nanostructured Al2024–multiwall carbon nanotubes (MWCNTs) composites were produced using optimized mechanical milling and hot pressing methods. Nanostructured Al2024 powder was first prepared through 30 h mechanical milling of the alloy powder. MWCNTs up to 3 vol.% were added to the milled Al2024 powder and milled for different times. Differential thermal analysis (DTA) and X-ray diffraction (XRD) were used to assess the structural changes and thermal behavior during mechanical milling and hot pressing. Hardness and compression tests were applied on bulk samples to evaluate their mechanical properties. Mechanical milling applied on Al2024 powders for 30 h resulted in the grain refinement to ～30 nm. DTA analysis showed an endothermic peak at ～632 °C due to Al2024 melting and an exothermic peak between 645 and 658 °C related to Al and MWCNTs reaction. Mechanical milling of nanocomposite powder for 4 h and following hot pressing at 500 °C under a pressure of 250 MPa for 0.5 h were selected as optimized conditions for bulk nanocomposite preparation. With MWCNTs addition up to 2 vol.%, relative density remained at 98%, and hardness increased to 245 HV. Compressive strength of nanocomposites found a maximum value of 810 MPa at 2 vol.% MWCNTs addition which is 78%, 34% and 12% greater than that for Al2024–O, Al2024–T6 and nanostructured Al2024, respectively.     

Mechanical alloying and spark plasma sintering of CoCrFeNiMnAl high-entropy alloy

An equiatomic CoCrFeNiMnAl high-entropy alloy was synthesized by mechanical alloying, and alloying behaviors, microstructure and annealing behaviors were investigated. It was found that a solid solution with refined microstructure of 20 nm in grain size could be obtained after 30 h milling. As-milled powder transformed into a face-centered cubic phase above 500 °C. The as-milled powder was subsequently consolidated by spark plasma sintering at 800 °C, BCC phase and FCC phase coexisted in the consolidated HEA, which had excellent properties in Vickers hardness of 662 HV and compressive strength of 2142 MPa.     

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.     

Dry sliding tribological behavior and mechanical properties of Al2024–5 wt.%B4C nanocomposite produced by mechanical milling and hot extrusion

In this paper, tribological behavior and mechanical properties of nanostructured Al2024 alloy produced by mechanical milling and hot extrusion were investigated before and after adding B₄C particles. Mechanical milling was used to synthesize the nanostructured Al2024 in attrition mill under argon atmosphere up to 50 h. A similar process was used to produce Al2024–5 wt.%B₄C composite powder. The milled powders were formed by hot pressing and then were exposed to hot extrusion in 750 °C with extrusion ratio of 10:1. To study the microstructure of milled powders and hot extruded samples, optical microscopy, transmission electron microscopy and scanning electron microscopy (SEM) equipped with an energy dispersive X-ray spectrometer (EDS) were used. The mechanical properties of samples were also compared together using tension, compression and hardness tests. The wear properties of samples were studied using pin-on-disk apparatus under a 20 N load. The results show that mechanical milling decreases the size of aluminum matrix grains to less than 100 nm. The results of mechanical and wear tests also indicate that mechanical milling and adding B₄C particles increase strength, hardness and wear resistance of Al2024 and decrease its ductility remarkably.     

Mechanical alloying and sintering of nanostructured TiO2 reinforced copper composite and its characterization

Mechanical alloying is a suitable method for producing copper based composites. Cu–TiO₂ composite was fabricated using high energy ball milling and conventional consolidation. Ball milling was performed at different milling durations (0–24 h) to investigate the effects of the milling time on the formation and properties of produced nanostructured Cu–TiO₂ composites. The amount of the TiO₂ in the final composition of the composite assumed to be 0, 1, 3, 5 and 7 wt%. The milled composite powders were characterized by X-ray diffraction, scanning electron microscopy and transmission electron microscopy to investigate the effects of the milling time on the formation of the composite and its properties. Also hardness, density and electrical conductivity of the sintered specimen were measured. High energy ball milling causes a high density of defects in the powders. Thus the Cu crystallite size decreases, generally to less than 50 nm. The maximum hardness value (105 HV) of the sintered compacts belongs to Cu–5 wt%TiO₂ which has been milled for 12 h.     

Synthesis of Ti-based bulk quasicrystal by shock compression

We attempted to produce a Ti₄₅Zr₃₈Ni₁₇ bulk icosahedral (i) quasicrystal by a shock compression technique, in which a single-stage powder gun discharges a flyer plate that consolidates the target powders. The results were also compared with those by a conventional hot-pressing. The powder mixtures for the shock compression were blended by two kinds of methods; that is, gently mixing in a vial, and mechanically alloying by a planetary ball mill. A large bulk i-phase sample, with a Ti₂Ni crystal phase, was synthesized from mechanically alloyed powders after shock compression at a higher flyer velocity, although the conventional hot-pressing at 3 MPa synthesized only the Ti₂Ni phase. For the gently mixed powders, no reaction occured even after shock compression. High-pressure and high-temperature produced during shock compression, and milling process were key factors to obtain the i-phase. The Vickers hardness and the wetting contact angle with pure water under an atmospheric pressure for the bulk sample containing the i-phase were about 7 GPa and about 70°, respectively.     

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.     

Microstructural and mechanical characteristics of Cu–Cu2O composites compacted with pulsed electric current sintering and hot isostatic pressing

This paper reports the influence of applied sintering process – pulsed electric current sintering (PECS) and hot isostatic pressing (HIP) – on the microstructure and mechanical properties of Cu–Cu₂O composites. In PECS fine-grained structure was obtained while in HIPing the grain growth was more noticeable, mostly due to the longer process time. The studies also showed that Cu₂O-phase distributed in Cu-matrix increased microhardness; at a fixed grains size Cu–Cu₂O structure had higher hardness than Cu so that 20% higher microhardness was obtained when Cu₂O was doubled from 19.1 to 37.2 vol%. At best, 99.1% density with 690 nm grain size and 1.35 GPa hardness were achieved by PECS whereas by HIP the same density with 1860 nm grain size gave 1.02 GPa hardness. The grain growth and the effect of second phase clustering on the grain growth were evaluated experimentally.     

Synthesis and characterization of xTiO2(1 − x)α-Fe2O3 magnetic ceramic nanostructure system

Rutile-doped hematite xTiO₂(1 ? x)α-Fe₂O₃ (x = 0.0–1.0) nanostructures were synthesized using mechanochemical activation by ball milling. Their complex structural, magnetic and thermal properties were characterized by X-ray diffraction, Mössbauer spectroscopy and simultaneous DSC–TGA. XRD patterns yielded the dependence of lattice parameters and grain size as a function of ball milling time. For the molar concentrations x = 0.1 and 0.3, the Mössbauer spectra were fitted with one, two, three or four sextets, corresponding to the degree of Ti ion substitution of Fe ions in hematite lattice. After 12 h of ball milling, the completion of Ti ion substitution of Fe ions in hematite lattice occurs for x = 0.1 and 0.3. For x = 0.5 and 0.7, Mössbauer spectra fitting required sextets and a quadrupole-split doublet, representing Fe ions substituting Ti ions in the rutile lattice. The completion of Fe ion substitution of Ti ions in rutile lattice was not observed, as indicated by XRD patterns and Mössbauer spectra for these two molar concentrations. Simultaneous DSC–TGA measurements revealed that the mechanochemical activation by ball milling has a strong effect on the thermal behavior of this nanostructure system. The enthalpy dropped dramatically after 2 h of milling time, indicating the strong solid–solid interactions between TiO₂ and α-Fe₂O₃ after ball milling. The change in weight loss of hematite was caused by the decrease of grain size and ion substitutions between Fe and Ti after mechanochemical activation.     

Fabrication of transparent mullite ceramic by spark plasma sintering from powders synthesized via sol–gel process combined with pulse current heating

Mullite nanopowders were synthesized by combining the advantages of the sol–gel process with the rapid synthesis provided by pulse current heating. The mullite ceramic with an infrared transmittance of 83–88% in the wavelength range from 2.5 to 4 μm with a fine grain size of 200 nm was obtained by spark plasma sintering at 1350 °C. Due to the high relative density and the small grain size, the hardness and toughness values of the sample reached 17.82 GPa and 3.6 MPa m^1/2, respectively. In contrast, when the mullite powders synthesized in a muffle furnace, an intermediate phase occurred so that the powder synthesis required high crystallization temperatures and resulted in agglomerated particles. Thus, the mullite ceramics required high temperatures for densification. As a result, the optical and mechanical properties of the ceramics were poor due to the low relative density and the elongated grain growth.     

Microstructural characteristics and mechanical properties of carbon nanotube reinforced aluminum alloy composites produced by ball milling

The influence of milling time on the structure, morphology and thermal stability of multi-walled carbon nanotubes (MWCNTs) reinforced EN AW6082 aluminum alloy powders has been studied. After structural and microstructural characterization of the mechanically milled powders micro- and nano-hardness of the composite powder particles were evaluated. The morphological and X-ray diffraction studies on the milled powders revealed that the carbon nanotubes (CNTs) were uniformly distributed and embedded within the aluminum matrix. No reaction products were detected even after long milling up to 50 h. Nanotubes became shorter in length as they fractured under the impact and shearing action during the milling process. A high hardness of about 436 ± 52 HV is achieved for the milled powders, due to the addition of MWCNTs, after milling for 50 h. The increased elastic modulus and nanohardness can be attributed to the finer grain size evolved during high energy ball milling and to the uniform distribution of hard CNTs in the Al-alloy matrix. The hardness values of the composite as well as the matrix alloy compares well with that predicted by the Hall–Petch relationship.     

Magnetic and structural properties of nanostructured (Fe65Co35)100−xCrx (x = 0, 10) powders prepared by mechanical alloying process

This work focuses on the preparation of nanostructured (Fe₆₅Co₃₅)_100−xCr_x (x = 0, 10) powders by mechanical alloying. The powders are milled for different milling times (up to 90 h). Characterizations of the milled powders were carried out by X-ray diffraction (XRD), scanning electron microscopy (SEM) and vibratory sample magnetometer (VSM). It was observed that the formation of bcc-FeCo and bcc-FeCoCr phases were completely accomplished after 60 and 90 h of milling, respectively. The grain size decreases and the microstrain increases with increasing the milling time. In the initial stages of milling (up to 15 h) for the (Fe₆₅Co₃₅)₉₀Cr₁₀ powders, the saturation magnetization (M_s) decreased but further milling (up to 90 h) increased the M_s. However, the trend for coercivity was different and three stages were observed. An initial increasing stage (up to 15 h of milling), followed by a reducing middle stage (up to 60 h of milling) and then again an increasing final stage (up to 90 h milling). Besides, for the same milling time of 90 h, the addition of 10 at.% of Cr to Fe₆₅Co₃₅ powders leads to higher coercivity and lower saturation magnetization.     

Microstructure and mechanical properties of bulk highly faulted fcc/hcp nanostructured cobalt microstructures

Nanostructured cobalt powders with an average particle size of 50 nm were synthesized using a polyol method and subsequently consolidated by spark plasma sintering (SPS). SPS experiments performed at 650 °C with sintering times ranging from 5 to 45 min under a pressure of 100 MPa, yielded to dense bulk nanostructured cobalt (relative density greater than 97%). X-ray diffraction patterns of the as-prepared powders showed only a face centered cubic (fcc) crystalline phase, whereas the consolidated samples exhibited a mixture of both fcc and hexagonal close packed (hcp) phases. Transmission electron microscopy observations revealed a lamellar substructure with a high density of nanotwins and stacking faults in every grain of the sintered samples. Room temperature compression tests, carried out at a strain rate of 10^− 3 s^− 1, yielded to highest strain to fracture values of up to 5% for sample of holding time of 15 min, which exhibited a yield strength of 1440 MPa, an ultimate strength as high as 1740 MPa and a Young's modulus of 205 GPa. The modulus of elasticity obtained from the nanoindentation tests, ranges from 181 to 218 GPa. The lowest modulus value of 181 GPa was obtained for the sample with the highest sintering time (45 min), which could be related to mass density loss as a consequence of trapped gases releasing.