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In this study, Al-Al4C3 compounds were manufactured by mechanical milling followed by heat treatment. To analyze the microstructural evolution, the composites were sintered at 550 °C at different sintering times of 2, 4 and 6 h. The mechanical results suggest that dislocation density and crystallite size primarily contribute to hardening before the sintering process, with a minimal contribution from particle dispersion in this condition. The compound exhibited a significant 75% increase in hardness after 2 h of sintering, primarily attributed to the nucleation and growth of Al4C3 nanorods. The HRTEM analysis, combined with geometric phase analysis (GPA) at and near the Al-Al4C3 interface of the nanorods, revealed strain field distributions primarily associated with partial screw dislocations and the presence of closely spaced dislocation dipoles. These findings are consistent with the microstructural parameters determined from X-ray diffraction pattern analysis using the convolutional multiple whole profile (CMWP) method. This analysis showed that the predominant dislocation character is primarily of the screw type, with the dislocation dipoles being closely correlated. Based on these results, it is suggested that samples with a lower weight percentage of reinforcement and longer sintering times may experience reduced brittleness in Al/Al4C3 composites. Strengthening contributions were calculated using the Langford–Cohen and Taylor equations. [ABSTRACT FROM AUTHOR]

Fe50Mn35Sn15 Heusler alloy, obtained by mechanical alloying, was subjected to larger milling times in the range of 30–50 h to study the phase stability and morphology. X-ray diffraction studies have shown that the milled samples crystallise in a disordered A2 structure. The A2 structure was found to be stable in the milling range studied, contrary to the computation studies performed on this composition. Using Rietveld refinements, the lattice parameter, mean crystallite size, and lattice strain were computed. The nature of the obtained phases by milling was found to be nanocrystalline with values below 50 nm. A linear increase rate of 0.00713 (h−1) was computed for lattice strain as the milling time increased. As the milling time increases, the lattice parameter of the cubic Heusler was found to have a decreasing behaviour, reaching 2.9517 Å at 50 h of milling. The morphological and elemental distribution—characterised by scanning electron microscopy and energy-dispersive X-ray spectroscopy—evidenced Mn and Sn phase clustering. As the milling time increased, the morphology of the sample was found to change. The Mn and Sn cluster size was quantified by elemental line profile. Electrical resistivity evolution with milling time was analysed, showing a peak for 40 h of milling time. [ABSTRACT FROM AUTHOR]

Ultrafine copper powders were prepared by the air-jet milling of copper oxide (CuO) powders and a subsequent hydrogen (H2) reduction. After milling, the particle size and grain size of CuO powders decreased, while the specific surface area and structural microstrain increased, thereby improving the reaction activity. In a pure H2 atmosphere, the process of CuO reduction was conducted in one step, and followed a pseudo-first-order kinetics model. The smaller CuO powders after milling exhibited higher reduction rates and lower activation energies compared with those without milling. Based on the unreacted shrinking core model, the reduction of CuO powders via H2 was controlled by the interface reaction at the early stage, whereas the latter was limited by the diffusion of H2 through the solid product layer. Additionally, the scanning electron microscopy (SEM) indicated that copper powders after H2 reduction presented a spherical-like shape, and the sintering and agglomeration between particles occurred after 300 °C, which led to a moderate increase in particle size. The preparing parameters (at 400 °C for 180 min) were preferred to obtain ultrafine copper powders with an average particle size in the range of 5.43–6.72 μm and an oxygen content of less than 0.2 wt.%. [ABSTRACT FROM AUTHOR]

Hot pressing represents a promising consolidation technique for ball-milled bismuth telluride alloys, yet deep investigations are needed to understand its effect on the thermoelectric properties. This paper studies the effect of hot-pressing parameters (temperature and pressure) on the thermoelectric properties of the n-type Gr-Bi2Te2.55Se0.45 nanocomposite. Ultra-high pressure, up to 1.5 GPa, is considered for the first time for consolidating Bi2(Te,Se)3 alloys. Results from this study show that increasing the temperature leads to changes in chemical composition and causes noticeable grain growth. On the contrary, increasing pressure mainly causes improvements in densification. Overall, increments in these two parameters improve the ZT values, with the temperature parameter having a higher influence. The highest ZT of 0.69 at 160 °C was obtained for the sample hot-pressed at 350 °C and 1 GPa for 5 min, which is indeed an excellent and competitive value when compared with results reported for this n-type Bi2Te2.55Se0.45 composition. [ABSTRACT FROM AUTHOR]

Improving the ductile deformation behavior of Mg-SiC nanocomposites without compromising strength is critical to enhancing their mechanical properties. Mg-SiC nanocomposites are produced through mechanical milling, cold isostatic pressing, sintering, and hot extrusion processes. This study investigates the uniaxial stress–strain response and deformation behavior of the Mg-SiC nanocomposite compared to pure Mg samples with and without the milling process. The deformation behavior was investigated by two-dimensional (2D) digital image correlation (DIC) at two macroscopic and microscopic scales, employing light micrographs and in situ loading samples, respectively, in the scanning electron microscope. Compared to the pure Mg samples, the mechanical test results demonstrated a significant improvement in strength (80 MPa) and fracture strain (23.5%) of the Mg-SiC nanocomposite. The three-dimensional (3D) representative volume element (RVE) model revealed the particle dispersion effect on the mechanical properties of the nanocomposite. The RVE results demonstrate ductile deformation behavior in the sample with homogenous dispersion of SiC particles compared with the heterogeneous dispersion of SiC particles in Mg-SiC nanocomposite. The results demonstrated a good agreement between DIC and RVE predictions for Mg-SiC nanocomposites across macro- and microscales. [ABSTRACT FROM AUTHOR]

The powder metallurgy (PM) route for the production of closed-cell metallic foams has recently received a significant amount of attention. One of the major issues is the non-uniform and non-spherical nature of the cells produced, which can negatively affect the mechanical behavior. The current paper uses the PM route to process metallic foams for the first time using novel Al-TiH2 foamable precursor "particles" (FPPs). The effect of FPP content (0–10 wt.%) on the developed foam structure of aluminum and its mechanical properties is investigated. An increase in FPP content results in a decline in product density by forming uniform and near-spherical cells. The main advantage of the FPPs is the localization of the blowing agent TiH2 particle content within Al-TiH2 composite particles (i.e., giving rise to a higher local TiH2 content), which has led to the production of pores with relatively high circularities even at very low overall TiH2 contents. The foams produced displayed energy absorption capacities of 10–25 MJ/m3 at 50% strain, and maximum energy absorption efficiencies ranging from 0.6–0.7 (for 40–60% closed cell content) [ABSTRACT FROM AUTHOR]

Copper matrix composites with zirconium diboride (ZrB2) were synthesised by ball milling and consolidated by Spark Plasma Sintering (SPS). Characterisations of the ball-milled composite powders were performed by scanning electron microscopy (SEM), X-ray diffraction, and measurement of the particle size distribution. The effect of the sintering temperature (1123 K, 1173 K, and 1223 K) and pressure (20 MPa and 35 MPa) on the density, porosity, and Young's modulus was investigated. The relationship between the change of Orb content and physical, mechanical, and electrical properties was studied. Experimental data showed that the properties of Cu–Orb composites depended significantly on the SPS sintering conditions. The optimal sintering temperature was 1223 K with a pressure of 35 MPa. Composites exhibited a high degree of consolidation. For these materials, the apparent density was in the range of 93–97%. The results showed that the higher content of Orb in the copper matrix was responsible for the improvement in Young's modulus and hardness with the reduction of the conductivity of sintered composites. The results showed that Young's modulus and the hardness of the Cu 20% Orb composites were the highest, and were 165 GPa and 174 HV0.3, respectively. These composites had the lowest relative electrical conductivity of 17%. [ABSTRACT FROM AUTHOR]

Mineral trioxide aggregates (MTA) are commonly used as endodontic filling materials but suffer from a long setting time and tooth discoloration. In the present study, the feasibility of using barium titanate (BTO) for discoloration and a calcium chloride (CaCl2) solution to shorten the setting time was investigated. BTO powder was prepared using high-energy ball milling for 3 h, followed by sintering at 700–1300 °C for 2 h. X-ray diffraction was used to examine the crystallinity and crystalline size of the as-milled and heat-treated powders. MTA-like cements were then prepared using 20–40 wt.% BTO as a radiopacifier and solidified using a 0–30% CaCl2 solution. The corresponding radiopacity, diametral tensile strength (DTS), initial and final setting times, and discoloration performance were examined. The experimental results showed that for the BTO powder prepared using a combination of mechanical milling and heat treatment, the crystallinity and crystalline size increased with the increasing sintering temperature. The BTO sintered at 1300 °C (i.e., BTO-13) exhibited the best radiopacity and DTS. The MTA-like cement supplemented with 30% BTO-13 and solidified with a 10% CaCl2 solution exhibited a radiopacity of 3.68 ± 0.24 mmAl and a DTS of 2.54 ± 0.28 MPa, respectively. In the accelerated discoloration examination using UV irradiation, the color difference was less than 1.6 and significantly lower than the clinically perceptible level (3.7). This novel MTA exhibiting a superior color stability, shortened setting time, and excellent biocompatibility has potential for use in endodontic applications. [ABSTRACT FROM AUTHOR]

In this study, the synthesis of tungsten carbides in a copper matrix by spark plasma sintering (SPS) is conducted and the microstructure formation mechanisms of the composite materials are investigated. The reaction mixtures were prepared by the high-energy mechanical milling (MM) of W, C and Cu powders. The influence of the MM time and SPS temperature on the tungsten carbide synthesis in an inert copper matrix was analyzed. It was demonstrated that the milling duration is a critical factor for creating the direct contacts between the W and C reactants and increasing the reactive transformation degree. A WC–W2C–Cu composite was fabricated from the W–C–3Cu powder mixture milled for 10 min and subjected to SPS at a temperature of 980 °C for 5 min. The formation of unconventional microstructures with Cu-rich regions is related to inter-particle melting during SPS. The WC–W2C–Cu composite showed a promising combination of mechanical and functional properties: a hardness of 300 HV, an electrical conductivity of 24% of the International Annealed Copper Standard, a residual porosity of less than 5%, a coefficient of friction in pair with a WC-6Co counterpart of 0.46, and a specific wear rate of the material of 0.52 × 10−5 mm3 N−1 m−1. [ABSTRACT FROM AUTHOR]

The interest in studying the synthesis of an Al–Cr alloy system by non-equilibria processes is due to the formation of metastable or quasicrystalline phases when rapid solidification has been utilized. Similarly, the formation of quasicrystals has been reported to a much lesser extent when the mechanical alloying technique was applied. In the present research, a mixture of powders of Cr and Al (both elements with a purity of 99.99%) with compositions of Al-5 and 7.5 at. % Cr was subjected to a ball milling process. Afterwards, the powder mixture was subjected to a consolidation process, conducted by pressing and sintering processes. The X-ray diffraction analyses revealed that during 20 h of milling there was no formation of metastable or quasicrystalline second phases detected. In addition, the X-ray diffraction peaks revealed that as milling time increased, the nanometric grain size decreased, and once the sintering treatment was applied, the crystallite size decreased following the same tendency. The dislocation density was estimated using the size of nanometric grains; this computation revealed that the dislocation density grew throughout the ball milling process; even after sintering, the multiplication of dislocations prevailed following the same tendency. [ABSTRACT FROM AUTHOR]

This review aims to expose mechanical milling as an alternative method for generating copper-based particles (copper particles (CuP) and copper composites (CuC)); more specifically, via a top-down or bottom-up approach, on a lab-scale. This work will also highlight the different parameters that can affect the size distribution, the type, and the morphology of the obtained CuP or CuC, such as the type of mechanical mill, ball-to-powder ratios (BPR), the milling speed, milling time, and the milling environment, among others. This review analyzes various papers based on the Cu-based particle generation route, which begins with a pretreatment step, then mechanical milling, its approach (top-down or bottom-up), and the post-treatment. Finally, the characterization methods of the resulting CuP and CuC through mechanical milling are also discussed. [ABSTRACT FROM AUTHOR]

A severe plastic deformation process for the achievement of favorable mechanical properties for metallic powder is mechanical milling. However, to obtain the highest productivity while maintaining reasonable manufacturing costs, the process parameters must be optimized to achieve the best mechanical properties. This study involved the use of response surface methodology to optimize the mechanical milling process parameters of harmonic-structure pure Cu. Certain critical parameters that affect the properties and fracture mechanisms of harmonic-structure pure Cu were investigated and are discussed in detail. The Box–Behnken design was used to design the experiments to determine the correlation between the process parameters and mechanical properties. The results show that the parameters (rotation speed, mechanical milling time, and powder-to-ball ratio) affect the microstructure characteristics and influence the mechanical performance, including the fracture mechanisms of harmonic-structure pure Cu specimens. The best combination values of the ultimate tensile strength (UTS) and elongation were found to be 272 MPa and 46.85%, respectively. This combination of properties can be achieved by applying an optimum set of process parameters: a rotation speed of 200 rpm; mechanical milling time of 17.78 h; and powder-to-ball ratio of 0.065. The superior UTS and elongation of the harmonic-structure pure Cu were found to be related to the delay of void and crack initiation in the core and shell interface regions, which in turn were controlled by the degree of strength variation between these regions. [ABSTRACT FROM AUTHOR]

Mineral trioxide aggregates (MTA) have been widely used in endodontic treatments, but after some time, patients suffer tooth discoloration due to the use of bismuth oxide (Bi2O3) as a radiopacifier. Replacement of Bi2O3 with high energy ball-milled single (zirconia ZrO2; hafnia, HfO2; or tantalum pentoxide, Ta2O5) or binary oxide powder was attempted, and corresponding discoloration improvement was investigated in the present study. Bi2O3-free MTA is expected to exhibit superior discoloration. The radiopacity, diametral tensile strength, and discoloration of MTA-like cements prepared from the as-milled powder were investigated. Experimental results showed that MTA-like cements prepared using Ta2O5 exhibited a slightly higher radiopacity than that of HfO2 but had a much higher radiopacity than ZrO2. Milling treatment (30 min to 3 h) did not affect the radiopacities significantly. These MTA-like cements exhibited superior color stability (all measured ΔE00 < 1.0) without any perceptible differences after UV irradiation. MTA-like cements prepared using ZrO2 exhibited the best color stability but the lowest radiopacity, which can be improved by introducing binary oxide. Among the investigated samples, MTA-like cement using (ZrO2)50(Ta2O5)50 exhibited excellent color stability and the best overall performance with a radiopacity of 3.25 mmAl and a diametral tensile strength of 4.39 MPa. [ABSTRACT FROM AUTHOR]

In this work, we demonstrate the possibility of using a soluble ceramic material, 5 wt% CaO, as an additive for an SmCo5/20wt%Fe exchange-coupled nanocomposite obtained by mechanical milling in order to inhibit the grain growth of the soft magnetic phase during annealing, which results in a more stable microstructure and an implicit improvement in the hard–soft interphase exchange coupling. Moreover, we show that the additive improves the phase stability of the composite material, reducing the amount of Sm2Co17-type phases formed during the synthesis process, an important aspect because Sm2Co17 is detrimental to the magnetic performance of the SmCo5/20%Fe nanocomposite. These effects are reflected in a nearly 13% increase in the coercive field (Hc) and a 20% increase in the energy product, (BH)max, for the powders produced using CaO as compared to pure SmCo5/20%Fe nanocomposites processed in the same manner. [ABSTRACT FROM AUTHOR]

The present work deals with powder metallurgical processing of Sn-reinforced Al-Cu-Fe icosahedral quasicrystalline (IQC) composites processed through mechanical milling (MM) followed by hot pressing and pressureless sintering. The structure, microstructure and toughening behavior of the nanocomposite powders and bulk samples were investigated through X-ray diffraction (XRD), optical metallography (OM), scanning electron microscopy (SEM) and indentation techniques. The XRD pattern suggested the coexistence of IQC and λ-Al13Fe4 (mC102; a = 1.549 nm, b = 0.808 nm, c = 1.248 nm) and B2-type Al (Cu, Fe) (cP2; a = 0.29 nm) crystalline phases in milled as well as sintered samples. The face-centered icosahedral (FCI) ordering was persistent even after 40 h of milling and sintering. The structural transformation during MM influences the indentation behavior of IQC-Sn nanocomposite powders, and the microhardness was found to be in the range of ~5.3 to 7.3 GPa. Further, efforts were made to study the indentation behavior of IQC-Sn composite prepared by pressureless sintering and hot pressing. The fracture toughness of the IQC-10Sn hot-pressed sample was found to be ~1.92 MPa. √ m , which is ~22% higher than that of the as-cast and annealed IQC. The enhancement in the fracture toughness resulted mainly from the inhibition of cracks by Sn reinforcement particles. This suggests that powder metallurgical processing can produce the IQC-Sn composite with an optimal combination of microhardness and fracture toughness. [ABSTRACT FROM AUTHOR]

Aluminium matrix composites (AlMCs) of AA7075 aluminium alloy reinforced with 0.5 and 1 wt.% multiwall carbon nanotubes (MWCNTs) were fabricated with powder metallurgy techniques using three different mechanical milling strategies, varying the milling energy and the stage in which the reinforcements were added to the pre-alloyed matrix powders. In this paper, we focus on the influence of these parameters on the dispersion of MWCNTs. Characterization of the obtained composite powders by X-ray diffraction and scanning electron microscopy showed that the evolution of the particle size and morphology of the composite powders is influenced by milling conditions and MWCNT content; however, under the conditions tested in this study, there were no significant differences in crystallite size and lattice strain. The best distribution of the reinforcements was obtained after milling 7075 powders and MWCNTs in a high-energy cycle (HEBM), varying the rotation speed between 1200 and 1300 rpm. Raman spectroscopy was used to assess the damage induced by the milling process in the nanotubes, and no reaction products were detected under any of the tested conditions. Nanoindentation tests were performed to measure the elastic modulus and hardness of the composite powders, revealing that the best mechanical behaviour was achieved by the 7075-0.5 wt.% MWCNT composites obtained by the HEBM route. [ABSTRACT FROM AUTHOR]

Although the dry ice method used to synthesize turbostratic carbon/graphene is little known and used, it has significant advantages over others, such as the following: it is low cost, simple, and a large quantity of material can be obtained using some inorganic and highly available acids (which can be reused). Despite the above advantages, the main reason for its incipient development is the resulting presence of magnesium oxide in the final product. In the present work, three different treatments were tested to remove this remnant using some acid chemical leaching processes, including hydrochloric acid, aqua regia, and piranha solution. Based on the experimental evidence, it was determined that using aqua regia and combining the leaching process with mechanical milling was the most efficient way of removing such a remnant, the residue being only 0.9 wt.%. This value is low compared to that obtained with the other acid leaching solutions and purification processes (2.8–29.6 wt.%). A mandatory high-energy mechanical milling stage was necessary during this treatment to expose and dissolve the highly insoluble oxide without secondary chemical reactions on the turbostratic carbon. High-energy mechanical milling is an effective route to exfoliate graphite, which allows the magnesium oxide to be more susceptible to acid treatment. A yield of turbostratic carbon/graphene of 1 wt.% was obtained from the metallic Mg. The obtained surface area was 504.8 m2g−1; this high value resulting from the intense exfoliation can potentiate the use of this material for a wide variety of applications. [ABSTRACT FROM AUTHOR]

In this study, a nano-composite material of a nanostructured Al-based matrix reinforced with Fe40Al intermetallic particles was produced by ball milling. During the non-equilibria processing, the powder mixtures with the compositions of Al-XFe40Al (X = 5, 10, and 15 vol. %) were mechanically milled under a low energy regime. The processed Al-XFe40Al powder mixtures were subjected to uniaxial pressing at room temperature. Afterward, the specimens were subjected to a sintering process under an inert atmosphere. In this thermal treatment, the specimens were annealed at 500 °C for 2 h. The sintering process was performed under an argon atmosphere. The crystallite size of the Al decreased as the milling time advanced. This behavior was observed in the three specimens. During the ball milling stage, the powder mixtures composed of Al-XFe40Al did not experience a mechanochemical reaction that could lead to the generation of secondary phases. The crystallite size of the Al displayed a predominant tendency to decrease during the ball milling process. The microstructure of the consolidated specimens indicated a uniform dispersion of the intermetallic reinforcement phases in the Al matrix. Moreover, according to the Vickers microhardness tests, the hardness varied linearly with the increase in the concentration of the Fe40Al intermetallic phase present in the composite material. The presented graphs indicate that the hardness increased almost linearly with the increasing dislocation density and with the reduction in grain sizes (both occurring during the non-equilibria processing). The microstructural and mechanical properties reported in this paper provide the aluminum matrix composite materials with the ideal conditions to be considered candidates for applications in the automotive and aeronautical industries. [ABSTRACT FROM AUTHOR]

The control of a homogeneous distribution of the reinforcing phase in aluminum matrix composites is the main issue during the synthesis of this kind of material. In this work, 2024 aluminum matrix composites reinforced with boron carbide were produced by mechanical milling, using 1 and 2 h of milling. After milling, powdered samples were cold consolidated, sintered and T6 heat treated. The morphology and microstructure of Al2024/B4C composites were investigated by scanning electron microscopy; analysis of X-ray diffraction peaks were used for the calculation of the crystallite size and microstrains by the Williamson-Hall method. The mechanical properties were evaluated by compression and hardness tests. B4C particles were found to be well dispersed into the aluminum matrix as a result of the high-energy milling process. The crystallite size of composites milled for 2 h was lower than those milled for 1 h. The hardness, yield strength and maximum strength were significantly improved in the composites processed for 2 h, in comparison to those processed for 1 h and the monolithic 2024 alloy. [ABSTRACT FROM AUTHOR]

The microstructure, phase composition, and microhardness of both gas-atomized and mechanically milled powders of the Al7075 + 1 wt % Zr alloy were investigated. The gas-atomized powder exhibited a cellular microstructure (grain size of a few µm) with layers of intermetallic phases along the cell boundaries. Mechanical milling (400 revolutions per minute (RPM)/8 h) resulted in a grain size reduction to the nanocrystalline range (20 to 100 nm) along with the dissolution of the intermetallic phases. Milling led to an increase in the powder's microhardness from 97 to 343 HV. Compacts prepared by spark plasma sintering (SPS) exhibited negligible porosity. The grain size of the originally gas-atomized material was retained, but the continuous layers of intermetallic phases were replaced by individual particles. Recrystallization led to a grain size increase to 365 nm in the SPS compact prepared from the originally milled powder. Small precipitates of the Al3Zr phase were observed in the SPS compacts, and they are believed to be responsible for the retainment of the sub-microcrystalline microstructure during SPS. A more intensive precipitation in this SPS compact can be attributed to a faster diffusion due to a high density of dislocations and grain boundaries in the milled powder. [ABSTRACT FROM AUTHOR]

This study focuses on the fabrication and microstructural investigation of Cu-TiH2-C and Cu-Ti-C nanocomposites with different volume fractions (10% and 20%) of TiC. Two mixtures of powders were ball milled for 10 h, consequently consolidated by spark plasma sintering (SPS) at 900 and 1000°C producing bulk materials with relative densities of 95-97%. The evolution process of TiC formation during sintering process was studied by using X-ray diffraction (XRD), scanning electron microscopy (SEM), and high resolution transmission electron microscopy (HRTEM). XRD patterns of composites present only Cu and TiC phases, no residual Ti phase can be detected. TEM images of composites with (10 vol % TiC) sintered at 900°C show TiC nanoparticles about 10-30 nm precipitated in copper matrix, most of Ti and C dissolved in the composite matrix. At the higher sintering temperature of 1000°C, more TiC precipitates from Cu-TiH2-C than those of Cu-Ti-C composite, particle size ranges from 10 to 20 nm. The hardness of both nanocomposites also increased with increasing sintering temperature. The highest hardness values of Cu-TiH2-C and Cu-Ti-C nanocomposites sintered at 1000°C are 314 and 306 HV, respectively. [ABSTRACT FROM AUTHOR]

Hot work tool steel (AISI H13) and high speed steel (AISI M3:2) powders were successfully co-sintered to produce hybrid tool steels that have properties and microstructures that can be modulated for specific applications. To promote co-sintering, which is made difficult by the various densification kinetics of the two steels, the particle sizes and structures were refined by mechanical milling (MM). Near full density samples (>99.5%) showing very fine and homogeneous microstructure were obtained using spark plasma sintering (SPS). The density of the blends (20, 40, 60, 80 wt % H13) was in agreement with the linear rule of mixtures. Their hardness showed a positive deviation, which could be ascribed to the strengthening effect of the secondary particles altering the stress distribution during indentation. A toughening of the M3:2-rich blends could be explained in view of the crack deviation and crack arrest exerted by the H13 particles. [ABSTRACT FROM AUTHOR]

Development of homogenous metal matrix nanocomposites with uniform distribution of nanoreinforcement, preserved matrix nanostructure features, and improved properties, was possible by means of innovative processing techniques. In this work, Al-SiC nanocomposites were synthesized by mechanical milling and consolidated through spark plasma sintering. Field Emission Scanning Electron Microscope (FE-SEM) with Energy Dispersive X-ray Spectroscopy (EDS) facility was used for the characterization of the extent of SiC particles' distribution in the mechanically milled powders and spark plasma sintered samples. The change of the matrix crystallite size and lattice strain during milling and sintering was followed through X-ray diffraction (XRD). The density and hardness of the developed materials were evaluated as function of SiC content at fixed sintering conditions using a densimeter and a digital microhardness tester, respectively. It was found that milling for 24 h led to uniform distribution of SiC nanoreinforcement, reduced particle size and crystallite size of the aluminum matrix, and increased lattice strain. The presence and amount of SiC reinforcement enhanced the milling effect. The uniform distribution of SiC achieved by mechanical milling was maintained in sintered samples. Sintering led to the increase in the crystallite size of the aluminum matrix; however, it remained less than 100 nm in the composite containing 10 wt.% SiC. Density and hardness of sintered nanocomposites were reported and compared with those published in the literature. [ABSTRACT FROM AUTHOR]

Mn-Al powders were prepared by rapid solidification followed by high-energy mechanical milling. The rapid solidification resulted in single-phase ε. The milling was performed in both the ε phase and the τ phase, with the τ-phase formation accomplished through a heat treatment at 500 °C for 10 min. For the e-milled samples, the conversion of the ε to the τ phase was accomplished after milling via the same heat treatment. Mechanical milling induced a significant increase in coercivity in both cases, reaching 4.5 kOe and 4.1 kOe, respectively, followed by a decrease upon further milling. The increase in coercivity was the result of grain refinement induced by the high-energy mechanical milling. Additionally, in both cases a loss in magnetization was observed. Milling in the ε phase showed a smaller decrease in the magnetization due to a higher content of the τ phase. The loss in magnetization was attributed to a stress-induced transition to the equilibrium phases, as no site disorder or oxidation was observed. Surfactant-assisted milling in oleic acid also improved coercivity, but in this case values reached >4 kOe and remained stable at least through 32 h of milling. [ABSTRACT FROM AUTHOR]

MnAl is a promising rare-earth free permanent magnet for technological use. We have examined the effects of consolidation by back-pressure, assisted equal channel angular extrusion processing on mechanically-milled, gas-atomized Mn-46% at. Al powder. X-ray diffraction showed both that the extruded rod consisted mostly of metastable τ phase, with some of the equilibrium γ2 and β phases, and that it largely retained the as-milled nanostructure. Magnetic measurements show a coercivity of ≤4.4 kOe and a magnetization at 10 kOe of ≤40 emu/g. In addition, extrusions exhibit greater than 95% of the theoretical density. This study opens a new window in the area of bulk MnAl magnets with improved magnetic properties for technological use. [ABSTRACT FROM AUTHOR]

Silicon (Si)-based anode materials can increase the energy density of lithium (Li)-ion batteries owing to the high weight and volume capacity of Si. However, their electrochemical properties rapidly deteriorate due to large volume changes in the electrode resulting from repeated charging and discharging. In this study, we manufactured structurally stable Fe–Si alloy powders by performing high-energy milling for up to 24 h through the reduction of the Si phase size and the formation of the α-FeSi2 phase. The cause behind the deterioration of the electrochemical properties of the Fe–Si alloy powder produced by over-milling (milling for an increased time) was investigated. The 12 h milled Fe–Si alloy powder showed the best electrochemical properties. Through the microstructural analysis of the Fe–Si alloy powders after the evaluation of half/full coin cells, powder resistance tests, and charge/discharge cycles, it was found that this was due to the low electrical conductivity and durability of β-FeSi2. The findings provide insight into the possible improvements in battery performance through the commercialization of Fe–Si alloy powders produced by over-milling in a mechanical alloying process. [ABSTRACT FROM AUTHOR]

The formation and hydrogen sorption properties of the NaMgH3 perovskite/type hydride have been examined. Samples were mechanically ball milled under argon for 2, 5 and 15 h; then characterized by X-ray diffraction (XRD), differential scanning calorimetry (DSC), and thermogravimetric analysis (TGA) coupled with a mass spectrometer (MS). Lattice parameters and cell volume of the main NaMgH3 phase increase as a function of milling. Dehydrogenation proceeded in two-step reactions for the NaMgH3. The maximum amount of released hydrogen was achieved for the 2 h milled NaMgH3 hydride accounting for 5.8 wt.% of H2 from 287 °C to 408 °C. Decomposed NaMgH3 samples were reversibly hydrogenated under 10 bar H2 at ~200 °C. [ABSTRACT FROM AUTHOR]

Commercially pure (c.p.) titanium grade IV with a bimodal microstructure is a promising material for biomedical implants. The influence of the processing parameters on the physical, microstructural, and mechanical properties was investigated. The bimodal microstructure was achieved from the blends of powder particles with different sizes, while the porous structure was obtained using the space-holder technique (50 vol.% of ammonium bicarbonate). Mechanically milled powders (10 and 20 h) were mixed in 50 wt.% or 75 wt.% with c.p. titanium. Four different mixtures of powders were precompacted via uniaxial cold pressing at 400 MPa. Then, the specimens were sintered at 750 °C via hot pressing in an argon gas atmosphere. The presence of a bimodal microstructure, comprised of small-grain regions separated by coarse-grain ones, was confirmed by optical and scanning electron microscopies. The samples with a bimodal microstructure exhibited an increase in the porosity compared with the commercially available pure Ti. In addition, the hardness was increased while the Young's modulus was decreased in the specimens with 75 wt.% of the milled powders (20 h). [ABSTRACT FROM AUTHOR]

Li-ion batteries are widely used as energy storage devices due to their excellent electrochemical performance. The cubic Li7La3Zr2O12 (c-LLZO) compound is regarded as a promising candidate as a solid-state electrolyte for lithium-ion batteries due to its high bulk Li-ion conductivity, excellent thermal performance, and chemical stability. The standard manufacturing procedure involves the high-temperature and lengthy annealing of powders. However, the formation of the tetragonal modification of LLZO and other undesired side phases results in the deterioration of electrochemical properties. The mechanical milling of precursor powders can enhance the powders' reactivity and can result in an easier formation of c-LLZO. The aim of this work was to study the influence of selected milling and annealing parameters on c-LLZO compound formation. The starting powders of La(OH)3, Li2CO3, and ZrO2 were subjected to milling in various ball mills, under different milling conditions. The powders were then annealed at various temperatures for different lengths of times. These studies showed that the phase transformation processes of the powders were not very sensitive to the milling parameters. On the other hand, the final phase composition and microstructure strongly depended on heat treatment conditions. Low temperature annealing (750 °C) for 3 h produced 90% of c-LLZO in the powder structure. [ABSTRACT FROM AUTHOR]

Among the various phases of bismuth oxide, the high temperature metastable face-centered cubic δ phase attracts great attention due to its unique properties. It can be used as an ionic conductor or an endodontic radiopacifying material. However, no reports concerning tantalum and bismuth binary oxide prepared by high energy ball milling and serving as a dental radiopacifier can be found. In the present study, Ta2O5-added Bi2O3 composite powders were mechanically milled to investigate the formation of these metastable phases. The as-milled powders were examined by X-ray diffraction and scanning electron microscopy to reveal the structural evolution. The as-milled composite powders then served as the radiopacifier within mineral trioxide aggregates (i.e., MTA). Radiopacity performance, diametral tensile strength, setting times, and biocompatibility of MTA-like cements solidified by deionized water, saline, or 10% calcium chloride solution were investigated. The experimental results showed that subsequent formation of high temperature metastable β-Bi7.8Ta0.2O12.2, δ-Bi2O3, and δ-Bi3TaO7 phases can be observed after mechanical milling of (Bi2O3)95(Ta2O5)5 or (Bi2O3)80(Ta2O5)20 powder mixtures. Compared to its pristine Bi2O3 counterpart with a radiopacity of 4.42 mmAl, long setting times (60 and 120 min for initial and final setting times) and 84% MG-63 cell viability, MTA-like cement prepared from (Bi2O3)95(Ta2O5)5 powder exhibited superior performance with a radiopacity of 5.92 mmAl (the highest in the present work), accelerated setting times (the initial and final setting time can be shortened to 25 and 40 min, respectively), and biocompatibility (94% cell viability). [ABSTRACT FROM AUTHOR]

The aim of this study is to synthesize Li1+xAlxTixSn2−2x(PO4) sodium super ion conductor (NASICON) -based ceramic solid electrolyte and to study the effect of dual metal substitution on the electrical and structural properties of the electrolyte. The performance of the electrolyte is analyzed based on the sintering temperature (550 to 950 °C) as well as the composition. The trend of XRD results reveals the presence of impurities in the sample, and from Rietveld Refinement, the purest sample is achieved at a sintering temperature of 950 °C and when x = 0.6. The electrolytes obey Vegard′s Law as the addition of Al3+ and Ti4+ provide linear relation with cell volume, which signifies a random distribution. The different composition has a different optimum sintering temperature at which the highest conductivity is achieved when the sample is sintered at 650 °C and x = 0.4. Field emission scanning electron microscope (FESEM) analysis showed that higher sintering temperature promotes the increment of grain boundaries and size. Based on energy dispersive X-ray spectroscopy (EDX) analysis, x = 0.4 produced the closest atomic percentage ratio to the theoretical value. Electrode polarization is found to be at maximum when x = 0.4, which is determined from dielectric analysis. The electrolytes follow non-Debye behavior as it shows a variety of relaxation times. [ABSTRACT FROM AUTHOR]

Commercially pure (c.p.) titanium grade IV with a bimodal microstructure is a promising material for biomedical implants. The influence of the processing parameters on the physical, microstructural, and mechanical properties was investigated. The bimodal microstructure was achieved from the blends of powder particles with different sizes, while the porous structure was obtained using the space-holder technique (50 vol.% of ammonium bicarbonate). Mechanically milled powders (10 and 20 h) were mixed in 50 wt.% or 75 wt.% with c.p. titanium. Four different mixtures of powders were precompacted via uniaxial cold pressing at 400 MPa. Then, the specimens were sintered at 750 °C via hot pressing in an argon gas atmosphere. The presence of a bimodal microstructure, comprised of small-grain regions separated by coarse-grain ones, was confirmed by optical and scanning electron microscopies. The samples with a bimodal microstructure exhibited an increase in the porosity compared with the commercially available pure Ti. In addition, the hardness was increased while the Young's modulus was decreased in the specimens with 75 wt.% of the milled powders (20 h).

By superposition, the individual strengthening mechanisms via hardness analyses and the particle dispersion contribution to strengthening were estimated for Al–C and Al–C–Cu composites and pure Al. An evident contribution to hardening due to the density of dislocations was observed for all samples; the presence of relatively high-density values was the result of the difference in the coefficients of thermal expansion (CTE) between the matrix and the reinforced particles when the composites were subjected to the sintering process. However, for the Al–C–Cu composites, the dispersion of the particles had an important effect on the strengthening. For the Al–C–Cu composites, the maximum increase in microhardness was ~210% compared to the pure Al sample processed under the same conditions. The crystallite size and dislocation density contribution to strengthening were calculated using the Langford–Cohen and Taylor equations from the microstructural analysis, respectively. The estimated microhardness values had a good correlation with the experimental. According to the results, the Cu content is responsible for integrating and dispersing the Al4C3 phase. The proposed mathematical equation includes the combined effect of the content of C and Cu (in weight percent). The composites were fabricated following a powder metallurgical route complemented with the mechanical alloying (MA) process. Microstructural analyses were carried out through X-ray analyses coupled with a convolutional multiple whole profile (CMWP) fitting program to determine the crystallite size and dislocation density. [ABSTRACT FROM AUTHOR]

In this work, vanadium particles (VP) were utilized as a novel reinforcement of AZ31 magnesium (Mg) alloy. The nanocrystalline (NC) AZ31–VP composites were prepared via mechanical milling (MM) and vacuum hot-press sintering. During the milling process, the presence of VP contributed to the cold welding and fracture mechanism, resulting in the acceleration of the milling process. Additionally, increasing the VP content accelerated the grain refinement of the matrix during the milling process. After milling for 90 h, the average grain size of AZ31-X wt % Vp (X = 5, 7.5, 10) was refined to only about 23 nm, 19 nm and 16 nm, respectively. In the meantime, VP was refined to sub-micron scale and distributed uniformly in the matrix, exhibiting excellent interfacial bonding with the matrix. After the sintering process, the average grain size of AZ31-X wt % VP (X = 5, 7.5, 10) composites still remained at the NC scale, which was mainly caused by the pinning effect of VP. Besides that, the porosity of the sintered composites was no more than 7.8%, indicating a good densification effect. As a result, there was little difference between the theoretical and real density. Compared to as-cast AZ31 Mg alloy, the microhardness of sintered AZ31-X wt % VP (X = 5, 7.5, 10) composites increased by 65%, 87% and 96%, respectively, owing to the strengthening mechanisms of grain refinement strengthening, Orowan strengthening and load-bearing effects. [ABSTRACT FROM AUTHOR]

Aluminum powder with different C and C–Cu mixtures powders were fabricated by powder metallurgy, using high-energy mechanical milling as a pre-treatment of powders. To evaluate the combined effect of the C–Cu mixture and the process conditions, such as sintering temperature/time and milling time, on the yield stress and hardness, two experimental designs were carried out. The results were analyzed with Minitab Statistical Software using contour plots. From the results, better mechanical properties were found at a Cu/C ratio of 0.33 and samples with high C content (3 wt. %). In samples subject to long sintering time (3 h), the mechanism of precipitation of the second phase was mainly present, resulting in an improvement in mechanical properties. From the difference found between the elastic limit and the microhardness tests, it was found that there was an inefficient sintering process affecting the elastic limit test results. Additionally, X-ray analyses using the Rietveld program, were used for microstructural characterization and mechanical parameters of yield strength and ultimate tensile strength. [ABSTRACT FROM AUTHOR]

In this study, in situ Al2O3-reinforced Ti3Al composite was fabricated after 8 h of milling and sintering at 850 °C. A mixture of TiO2 and Al powders were mechanically milled in a planetary mill, cold-compacted and sintered under a protected argon atmosphere. The microstructure and microhardness of the Al2O3 embedded in Ti3Al matrix at both room and elevated temperature has been reported. The obtained results showed that the Ti3Al/Al2O3 composite was successfully synthesized via the powder metallurgy method. Ti3Al phase and Al2O3 particles were formed after 8 h of milling and sintering at 850 °C. The microstructure formation of round and uniformly distributed Al2O3 particles in the Ti3Al matrix improved the microhardness of the composite. At normal temperature, the microhardness of the material measured about 11.5 GPa. Meanwhile, at elevated temperatures, from 600 to 800 °C, it decreased from 4.18 GPa to 3.15 GPa. [ABSTRACT FROM AUTHOR]

The paper describes an attempt to obtain harmonic structure (HS) in AISI308L steel. Harmonic structure is the term related to the microstructure fabricated by mechanical milling of metallic powders under soft milling conditions, resulting in the formation of plastically deformed, grain-refined shell and unchanged core. This microstructure can be preserved after successful powder compaction. The powders of AISI308L steel were milled under soft condition up to 50 h and then compacted by pulse plasma sintering at 900–1100 °C. For powders and compacts XRD, SEM and hardness measurements were applied as characterization techniques. The milling process resulted in austenite transformation into nanocrystalline ferrite and formation of grain refined outer layer. The applied pulse plasma sintering parameters allowed preservation of this microstructure and manufacturing of compacts with homogeneous distribution of elements, relative density above 95% and hardness in the range 167–185 HV, depending on sintering temperature. Simultaneously, the starting phase composition was restored, i.e., austenite with 12% contribution of ferrite. The crystallite size of austenite was about 20 nm and was significantly smaller then in starting powders. [ABSTRACT FROM AUTHOR]

The aim of this study was to prepare a low porosity bulk sample with a fine-grained structure from an AlZrTi alloy. Nanostructured powder particles were prepared by mechanical milling of gas atomized powder. The mechanically milled powder was consolidated using spark plasma sintering technology at 475 °C for 6 min using a pressure of 100 MPa. Sintering led to a low porosity sintered sample with a bimodal microstructure. The sintered sample was revealed to be composed of non-recrystallized grains with an approximate size of about 100 nm encompassed by distinct clusters of coarser, micrometer-sized grains. Whereas the larger grains were found to be lean on second phase particles, a high density of second phase particles was found in the areas of fine grains. The microhardness of the milled powder particles was established to be 163 ± 15 HV0.01, which decreased to a slightly lower value of 137 ± 25 HV0.01 after sintering. [ABSTRACT FROM AUTHOR]

Nanostructured alloy powders of SmCo5 + 10 wt% Fe obtained using recycled material were studied for the first time. The SmCo5 precursor was obtained from commercial magnets recycled by hydrogen decrepitation. The results were compared with identically processed samples obtained using virgin SmCo5 raw material. The samples were synthesized by dry high-energy ball-milling and subsequent heat treatment. Robust soft/hard exchange coupling was observed—with large coercivity, which is essential for commercial permanent magnets. The obtained energy products for the recycled material fall between 80% and 95% of those obtained when using virgin SmCo5, depending on milling and annealing times. These results further offer viability of recycling and sustainability in production. These powders and processes are therefore candidates for the next generation of specialized and nanostructured exchange-coupled bulk industrial magnets. [ABSTRACT FROM AUTHOR]

In this work, nanocrystalline AZ31 magnesium alloy powders, reinforced by submicron TiB2 particles, were prepared via mechanical milling. It was found that TiB2 particles stimulated the fracture and welding of AZ31/TiB2 powders, leading to the acceleration of the milling process. Meanwhile, the TiB2 particles were refined to submicron-scale size during the milling process, and their distribution was uniform in the Mg matrix. In addition, the matrix was significantly refined during the milling process, which was also accelerated by the TiB2 particles. The formation of grain boundary segregation layers also led to the weakened TiB2 peaks in the XRD patterns during the mechanical milling. The grain sizes of AZ31–2.5 wt % TiB2, AZ31–5 wt % TiB2 and AZ31–10 wt % TiB2 powders were refined to 53 nm, 37 nm and 23 nm, respectively, after milling for 110 h. Under the combined effect of the nanocrystalline matrix and the well-dispersed submicron TiB2 particles, the AZ31/TiB2 composites exhibited excellent micro-hardness. For the AZ31–10 wt % TiB2 composite, the micro-hardness was enhanced to 153 HV0.5. [ABSTRACT FROM AUTHOR]

Mineral trioxide aggregate (MTA) typically consists of Portland cement (75 wt.%), bismuth oxide (20 wt.%), and gypsum (5 wt.%) and is commonly used as endodontic cement. Bismuth oxide serving as the radiopacifying material reveals the canal filling effect after clinical treatment. In the present study, bismuth/zirconium oxide composite powder was prepared by high energy ball milling of (Bi 2 O 3 ) 100 - x (ZrO 2 ) x (x = 5, 10, 15, and 20 wt.%) powder mixture and used as the radiopacifiers within MTA. The crystalline phases of the as-milled powders were examined by the X-ray diffraction technique. The radiopacities of MTA-like cements prepared by using as-milled composite powders (at various milling stages or different amount of zirconia addition) were examined. In addition, the stability of the as-milled powders stored in an ambient environment, an electronic dry box, or a glove box was investigated. The experimental results show that the as-milled powder exhibited the starting powder phases of Bi 2 O 3 and ZrO 2 and the newly formed δ-Bi 7.38 Zr 0.62 O 2.31 phase. The longer the milling time or the larger the amount of the zirconia addition, the higher the percentage of the δ-Bi 7.38 Zr 0.62 O 2.31 phase in the composite powder. All the MTA-like cements prepared by the as-milled powder exhibited a radiopacity higher than 4 mmAl that is better than the 3 mmAl ISO standard requirement. The 30 min as-milled (Bi 2 O 3 ) 95 (ZrO 2 ) 5 composite powder exhibited a radiopacity of 5.82 ± 0.33 mmAl and degraded significantly in the ambient environment. However, storing under an oxygen- and humidity-controlled glove box can prolong a high radiopacity performance. The radiopacity was 5.76 ± 0.08 mmAl after 28 days in a glove box that was statistically the same as the original composite powder., Competing Interests: The authors declare no conflict of interest.

High-temperature face-centered cubic bismuth oxide phase is a material of great interest given its unique properties. In the present study, α-Bi2O3 and tantalum powders were used as the starting powders for the formation of high-temperature bismuth oxide phase via mechanochemical synthesis by high energy ball milling. (Bi2O3)80(Ta)20 and (Bi2O3)95(Ta)5 in weight concentrations were milled in either an oxygen-free argon-filled glove box environment or an ambient atmosphere to investigate the effects of oxygen concentration and tantalum addition. The as-milled powders were examined using X-ray diffraction, scanning electron microscopy with energy-dispersive spectroscopy, and differential scanning calorimetry to reveal the structural evolution. The experimental results showed that for (Bi2O3)95(Ta)5 powder mixtures milled within the glove box, tantalum gradually reacted with the α-Bi2O3 phase and formed a β-Bi7.8Ta0.2O12.2 phase. For (Bi2O3)80(Ta)20 milled under the same conditions, Ta and α-Bi2O3 mechanochemically reacted to form δ-Bi3TaO7 and bismuth after 10 min of high energy ball milling, whereas milling (Bi2O3)80(Ta)20 under the ambient atmosphere with a much higher oxygen concentration accelerated the mechanochemical reaction to less than five minutes of milling and resulted in the formation of high-temperature δ-Bi3TaO7 phase. [ABSTRACT FROM AUTHOR]

The development of a magnesium matrix composite with a high content of dispersions using conventional liquid-phase process is a great challenge, especially for nanometer/submicron particles. In this work, mechanical milling was employed to prepare nanocrystalline AZ91 dispersed with 15 vol.% submicron SiC particles (SiCp/AZ91). AZ91 with no SiCp was applied as a comparative study with the same mechanical milling. In order to investigate the mechanism of dispersing, the morphology evolution of powders and the corresponding SiCp distribution were observed. As the scanning electron microscope (SEM) analysis exhibited, the addition of SiCp accelerated the smashing of AZ91 particles, which promoted the dispersion of SiCp in AZ91. Thus, after mechanical milling, 15 vol.% SiCp, which was smashed from 800 to 255 nm, got uniformly distributed in the Mg matrix. Based on X-ray diffraction (XRD) results, part of the Mg17Al12 precipitate got dissolved, and an Al-supersaturated Mg solid solution was formed. The transmission electron microscopy (TEM) results showed that the ultimate Mg grain (32 nm) of milled SiCp/AZ91 was much smaller than that of milled AZ91 (64 nm), which can be attributed to a pinning effect of submicron SiCp. After mechanical milling, the hardness of SiCp/AZ91 reached 185 HV, which was 185% higher than the original AZ91 and 33% higher than milled AZ91, due to fine Mg grain and submicron dispersions. [ABSTRACT FROM AUTHOR]

Mg97Zn1Y2 (at %) alloy with a long period stacking ordered (LPSO) phase has attracted a great deal of attention due to its excellent mechanical properties. It has been reported that this alloy could be fabricated by warm extrusion of rapid solidified alloy powders. In this study, an alternative route combining mechanical milling and equal channel angular pressing (ECAP) was selected to produce the bulk Mg97Zn1Y2 alloy. Microstructural characterization, mechanical properties and corrosion behavior of the ECAP-compacted alloys were studied. The as-cast alloy contained α-Mg and LPSO-Mg12Zn1Y1 phase. In the as-milled powder, the LPSO phase decomposed and formed Mg24Y5 phase. The ECAP-compacted alloy had identical phases to those of the as-milled sample. The compacted alloy exhibited a hardness of 120 HV and a compressive yield strength of 308 MPa, which were higher than those of the as-cast counterpart. The compacted alloy had better corrosion resistance, which was attributed to the reduced volume fraction of the secondary phase resulting in lower microgalvanic corrosion in the compacted alloy. The increase in Y content in the α-Mg matrix also contributed to the improvement of corrosion resistance. [ABSTRACT FROM AUTHOR]

Fine-grained W-6Ni-4Mn alloys were fabricated by spark plasma sintering (SPS) using mechanical milling W, Ni and Mn composite powders. The relative density of W-6Ni-4Mn alloy increases from 71.56% to 99.60% when it is sintered at a low temperature range of 1000–1200 °C for 3 min. The spark plasma sintering process of the alloy can be divided into three stages, which clarify the densification process of powder compacts. As the sintering temperature increases, the average W grain size increases but remains at less than 7 µm and the distribution of the binding phase is uniform. Transmission electron microscopy (TEM) observation reveals that the W-6Ni-4Mn alloy consists of the tungsten phase and the γ-(Ni, Mn, W) binding phase. As the sintering temperature increases, the Rockwell hardness and bending strength of alloys initially increases and then decreases. The optimum comprehensive hardness and bending strength of the alloy are obtained at 1150 °C. The main fracture mode of the alloys is W/W interface fracture. [ABSTRACT FROM AUTHOR]

The compact samples of an Al7075 alloy were prepared by a combination of gas atomization, high energy milling, and spark plasma sintering. The predominantly cellular morphology observed in gas atomized powder particles was completely changed by mechanical milling. The continuous-like intermetallic phases present along intercellular boundaries were destroyed; nevertheless, a small amount of Mg(Zn,Cu,Al)2 phase was observed also in the milled powder. Milling resulted in a severe plastic deformation of the material and led to a reduction of grain size from several µm into the nanocrystalline region. The combination of these microstructural characteristics resulted in abnormally high microhardness values exceeding 300 HV. Consolidation through spark plasma sintering (SPS) resulted in bulk samples with negligible porosity. The heat exposition during SPS led to precipitation of intermetallic phases from the non-equilibrium microstructure of both gas atomized and milled powders. SPS of the milled powder resulted in a recrystallization of the severely deformed structure. An ultra-fine grained structure (grain size close to 500 nm) with grains divided primarily by high-angle boundaries was formed. A simultaneous release of stored deformation energy and an increase in the grain size caused a drop of microhardness to values close to 150 HV. This value was retained even after annealing at 425 °C. [ABSTRACT FROM AUTHOR]