Synthesis and characterization of precipitation hardened amorphous matrix composite by mechanical alloying and pulse plasma sintering of Al65Cu20Ti15

This study reports synthesis of Al₆₅Cu₂₀Ti₁₅ amorphous alloy by mechanical alloying and consolidation of the powder mass by pulsed plasma sintering. During sintering, several intermetallic phases precipitate from the amorphous matrix and cause a significant increase in nano-hardness and elastic modulus. Microstructure in as-milled and sintered conditions was characterized by X-ray diffraction, scanning/transmission electron microscopy and differential scanning calorimetric. Among various conditions of sintering, the composites pulse plasma, sintered at 500°C, show the high compression strength (1745 MPa) and high indentation fracture toughness (4.96 MPa m^1/2); although, the maximum density (3.73 Mg/in³), nano-hardness (14 GPa) and Young's modulus (208 GPa) in the present alloy have been obtained in the composites pulse plasma sintered at 600°C.     

Effect of heat treatment on the mechanical and microstructural characterization of Mg-AZ91E/TiC composites

Mg-AZ91E/TiC_p composite was fabricated using a spontaneous infiltration technique at 950 °C under an argon atmosphere. The composites produced have 37 vol.% of metal matrix and 63 vol.% of TiC-like reinforcement. The obtained composites were subsequently solution heat-treated at 413 °C during 24 h, cold water quenched, and subsequently artificially aged at 168 and 216 °C during 16 h in an argon atmosphere. Effect of heat treatment on the microstructure and mechanical properties was evaluated. Microstructural characterization was analyzed using different techniques such as X-ray diffraction (XRD) and scanning electron microscopy (SEM). Interface between matrix and reinforcement was examined using transmission electron microscopy (TEM), and mechanical properties were evaluated by measuring the elastic modulus and hardness. Mg, TiC, Al, and Mg₁₇Al₁₂ phases through XRD were detected. Meanwhile, using TEM analysis in heat-treated composites MgAl₂O₄, MgO, and Al₂O₃ were identified. The as-fabricated composite have elastic modulus and hardness of 162 GPa and 316 Hv, respectively. After solution heat treatment and aging at 168 °C during 12 h, the composites reaches values of 178 GPa and 362 Hv for the elastic modulus and hardness, respectively. Time of aging was correlated with measures of elastic modulus and hardness.     

Factors affecting the microstructure and mechanical properties of Ti-Al3Ti core-shell-structured particle-reinforced Al matrix composites

This work studied the effects of matrix powder and sintering temperature on the microstructure and mechanical properties of in situ formed Ti–Al₃Ti core–shell-structured particle-reinforced pure Al-based composites. It has been shown that both factors have significant effects on the morphology of the reinforcements and densification behaviour of the composites. Due to the strong interfacial bonding and the limitation of the crack propagation in the intermetallic shell during deformation by soft Al matrix and Ti core, the composite fabricated using fine spherical-shaped Al powder and sintered at 570 °C for 5 h has the optimal combination of the overall mechanical properties. The study provides a direction for the optimum combination of high strength and ductility of the composites by adjusting the fabrication parameters.     

Reaction mechanisms between Al and Fe3O4 powders in the formation of an Al-based metal matrix composite

The reaction mechanisms between Al and Fe₃O₄ powders were investigated. Differential thermal analysis revealed that a two-step displacement reaction between Al and Fe₃O₄ took place during sintering. Initially, the Fe₃O₄ was converted to amorphous FeO at ～720°C and some of the Al was oxidized to amorphous Al₂O₃. In the final stage, when the temperature reached ～840°C, crystalline Al₂O₃ particles were produced in the molten Al–Fe liquid. The effects of cooling rate on the microstructures were studied. When the Al–Fe liquid was furnace-cooled to room temperature, proeutectic Al₃Fe plates, plate-like divorced eutectic Al₃Fe and Al₂O₃ particles were in situ formed in the Al(Fe) matrix. While quenching from 700°C, nanometer-sized Al dendrites and Al–Al₆Fe eutectic lamellae were produced in the Al matrix. However, when it was rapidly quenched from 900°C, the size of the proeutectic Al₃Fe phases was further reduced and Al₆Fe nanorods were found in the Al–Al₆Fe eutectics. A model was proposed to describe the transformation of the Al–Fe intermetallics during solidification.     

Microstructure and mechanical properties of nano-Y2O3 dispersed ferritic steel synthesized by mechanical alloying and consolidated by pulse plasma sintering

Ferritic steel with compositions 83.0Fe–13.5Cr–2.0Al–0.5Ti (alloy A), 79.0Fe–17.5Cr–2.0Al–0.5Ti (alloy B), 75.0Fe–21.5Cr–2.0Al–0.5Ti (alloy C) and 71.0Fe–25.5Cr–2.0Al–0.5Ti (alloy D) (all in wt%) each with a 1.0?wt% nano-Y₂O₃ dispersion were synthesized by mechanical alloying and consolidated by pulse plasma sintering at 600, 800 and 1000°C using a 75-MPa uniaxial pressure applied for 5?min and a 70-kA pulse current at 3?Hz pulse frequency. X-ray diffraction, scanning and transmission electron microscopy and energy disperse spectroscopy techniques have been used to characterize the microstructural and phase evolution of all the alloys at different stages of mechano-chemical synthesis and consolidation. Mechanical properties in terms of hardness, compressive strength, yield strength and Young's modulus were determined using a micro/nano-indenter and universal testing machine. All ferritic alloys recorded very high levels of compressive strength (850–2850?MPa), yield strength (500–1556?MPa), Young's modulus (175–250?GPa) and nanoindentation hardness (9.5–15.5?GPa), with up to 1–1.5 times greater strength than other oxide dispersion-strengthened ferritic steels (<1200?MPa). These extraordinary levels of mechanical properties can be attributed to the typical microstructure of uniform dispersion of 10–20-nm Y₂Ti₂O₇ or Y₂O₃ particles in a high-alloy ferritic matrix.     

Effects of sintering temperature and atmosphere on magnetism in Mn-doped TiO2 bulk samples

Magnetic properties have been investigated on Mn doped TiO₂(Ti_0.98Mn_0.02O₂) bulk samples prepared by solid state reaction, which were sintered at different temperature ranging from 450 ^°C to 900 ^°C in air and argon atmosphere, respectively. The results show that the magnetic properties were strongly dependent on the sintering temperature and atmosphere. For samples sintered in air, the magnetization initially increase with the increase of sintering temperature up to 600 ^°C and thereafter it decrease. While the magnetization of samples sintered in argon atmosphere decreases monotonically with the increase of sintering temperature. Furthermore, for samples sintered at 600 ^°C in air, the magnetic susceptibility exhibits a dominant Curie-Weiss behaviour and no magnetic transition is observed over the temperature range from 10 to 300 K. In contrast, for samples sintered in argon atmosphere, besides the magnetic transition near 45 K perhaps caused by Mn₃O₄, another magnetic transition appears near room temperature.     

Microstructure and mechanical properties of continuous Al2O3 fibre reinforced Ni45Al45Cr7.5Ta2.5 alloy (IP75) matrix composites

Single crystalline Al₂O₃ fibres (sapphire), coated with the NiAl alloy IP75 by physical vapour deposition (PVD), were assembled to fabricate composites by means of diffusion bonding. The microstructure and chemistry of both as-coated fibre and as-diffusion bonded composites were investigated by electron microscopy and microanalysis. The interface shear stress for complete debonding was measured by fibre push-out tests at room temperature, and the composite tensile strength was measured at 900°C and 1100°C. An amorphous layer with a thickness of about 400?nm formed between the fibre and the matrix during the PVD process and was maintained during diffusion bonding. A Laves phase precipitated along NiAl grain boundaries in the IP75 matrix. This caused a lower tensile strength of the IP75/Al₂O₃ composite at high temperatures compared to as-cast monolithic IP75 and rendered the composite useless for structural applications.     

Effect of low-temperature high-pressure sintering on BiFeO3 density,electrical magnetic and structural properties

Single-phase multiferroic BiFeO₃ (BFO) powders were prepared by hydrothermal microwave synthesis and dense BiFeO₃ ceramics were fabricated for the first time by the low-temperature high-pressure (LTHP) sintering technique. Effect of sintering temperature ranging from 400 to 800 °C (3 min and 10 min) and pressure of 3–8 GPa on structural, microstructural, electric and magnetic properties were investigated through X-ray diffraction, scanning electron microscope (SEM), electrochemical impedance spectroscopy (EIS), density and magnetic measurements. The results highlighted that LTHP sintering method, thanks to the high pressure involved, requires lower temperature and shorter time than other techniques, avoiding BiFeO₃ phase degradation. SEM images show that for short experimental time (t = 3 min) the average grain size of the sintered samples was approximately the same size of raw powder. Extending the sintering time up to 10 min the grain growth phenomena occurred. Moreover the results indicate that the best obtained density value was around 98% of theoretical density. The dielectric behavior of BiFeO₃ ceramics was not significantly influenced by the LTHP sintering conditions. Magnetic measurements showed that ceramic BiFeO₃ is weakly ferromagnetic at room temperature.     

Thermal properties and ionic conductivity of Li<Subscript>1,3</Subscript>Ti<Subscript>1,7</Subscript>Al<Subscript>0,3</Subscript>(PO<Subscript>4</Subscript>)<Subscript>3</Subscript> solid electrolytes sintered by field-assisted sintering

Li_1,3Ti_0,7Al_0,3(PO₄)₃ (LATP) powder was obtained by a conventional melt-quenching method and consolidated by field-assisted sintering technology (FAST) at different temperatures. Using this technique, the samples could be sintered to relative densities in the range of 93 to 99 % depending on the sintering conditions. Ionic and thermal conductivity were measured and the results are discussed under consideration of XRD and SEM analyses. Thermal conductivity values of 2 W/mK and ionic conductivities of 4?×?10^?4 Scm^?1 at room temperature were obtained using relatively large particles and a sintering temperature of 1000 °C at an applied uniaxial pressure of 50 MPa.     

Effect of calcination conditions on lithium conductivity in Li<Subscript>1.3</Subscript>Ti<Subscript>1.7</Subscript>Al<Subscript>0.3</Subscript>(PO<Subscript>4</Subscript>)<Subscript>3</Subscript> prepared by sol-gel route

In order to study the influence of powder calcination temperature on lithium ion conductivity, synthesized Li_1.3Ti_1.7Al_0.3(PO₄)₃ (LATP) was calcined at temperatures between 750 and 900 °C. The shape and size of the particles were characterized employing scanning electron microscopy (SEM), and specific surface area of the obtained powder was measured. The crystallinity grade of different heat-treated powders was calculated from XRD spectra. Posteriorly, all powders were sintered at 1100 °C employing field-assisted sintering (SPS), and the electrical properties were correlated to the calcination conditions. The highest ionic conductivity was observed for samples made out of powders calcined at 900 °C.     

Effect of sintering conditions on the properties of sol-gel-derived Li<Subscript>1.3</Subscript>Al<Subscript>0.3</Subscript>Ti<Subscript>1.7</Subscript>(PO<Subscript>4</Subscript>)<Subscript>3</Subscript>

Solid electrolyte Li_1.3Al_0.3Ti_1.7(PO₄)₃ was prepared by sol-gel method under different sintering conditions. The structural identification, surface morphology, electrochemical window, ionic conductivity, and activation energy of the Li_1.3Al_0.3Ti_1.7(PO₄)₃ sintered pellets were investigated by X-ray diffraction, scanning electron microscopy, cyclic voltammetry, and electrochemical impedance spectroscopy. It is found that the sintering temperature and time have considerable effect on the properties of the Li_1.3Al_0.3Ti_1.7(PO₄)₃ sintered pellets. The Li_1.3Al_0.3Ti_1.7(PO₄)₃ pellet sintered at 900 °C for 2 h is denser than the pellets sintered at other conditions. Different sintering conditions result in the sintered pellet with different porosity. However, the sintering conditions have little effect on the electrochemical window of Li_1.3Al_0.3Ti_1.7(PO₄)₃. Among the Li_1.3Al_0.3Ti_1.7(PO₄)₃ pellets sintered at various conditions, the pellet sintered at 900 °C for 2 h shows the highest ionic conductivity of 3.46 × 10⁻⁴ S cm⁻¹ and the lowest activation energy of 0.2821 eV.     

SEM and TEM analysis of composite of ZrO2-Ti system

3Y-ZrO₂-Ti composites obtained by slip casting method were studied by means of X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Moreover, the Vickers hardness was measured. The experiments show the complex microstructure of composites. The tetragonal zirconium dioxide (t-ZrO₂) and monoclinic zirconium dioxide (m-ZrO₂) as a composite matrix were detected at XRD analysis. SEM observations revealed that Ti -rich phase are uniform distributed in composites. Moreover, the large and very fine precipitations were found. The very fine Ti rich precipitations were located at ZrO₂ grain boundaries as well as in the triple-points. TEM experiments confirmed that in the sintered composites 3Y-ZrO₂ – 10%Ti the uniaxial ZrO₂ grains (100–600 nm), fine monoclinic martensitic plates and fine round monoclinic particles (20–40 nm) of ZrTiO₂ phase were exist. The complex microstructures of 3Y-ZrO₂-Ti composites have a high hardness as a result of existing fine ZrTiO₂ and other Ti oxides precipitations.     

Mechanical properties of kaolinite ‘macro-crystals’

The mechanical properties of a rare sample of kaolinite macroscopic crystals were evaluated using instrumented indentation. The crystals were also characterized by X-ray diffraction, scanning electron microscopy, atomic force microscopy and Fourier transform infrared spectroscopy before and after heat treatment at 1100°C. The results are explained in terms of the fracture process occurring in the layered structure of kaolinite, and of the effect of roughness on the hardness and elastic modulus. Data analysis using One-way ANOVA (p?<?0.05) showed that the values of hardness and elastic modulus obtained are statistically homogeneous. Before heat treatment, the sample was composed essentially of kaolinite, with hardness of 42?MPa and elastic modulus equal to 1.3?GPa. After calcination at 1100°C, the sample keeps its layered habit and consists of amorphous metakaolinite. The hardness increases to 360?MPa and the elastic modulus increases to 6.9?GPa.     

Preparation and characteristics of?a?BaO–Al2O3–B2O3–SiO2–La2O3 glass ceramic via spray pyrolysis

The characteristics of a BaO–Al₂O₃–B₂O₃–SiO₂–La₂O₃ glass ceramic prepared by spray pyrolysis were studied. Glass powders with spherical shape and amorphous phase were prepared by complete melting at a preparation temperature of 1 500°C. The mean size and geometric standard deviation of the powders prepared at the temperature of 1 500°C were 0.6 μm and 1.3. The glass powders had similar composition to that of the spray solution. The glass transition temperature (T _g) of the glass powders was 600.3°C. Two crystallization exothermic peaks were observed at 769.3 and 837.8°C. Densification of the specimen started at a sintering temperature of 600°C, in which Ba₄La₆O(SiO₄)₆ as main crystal structure was observed. Complete densification of the specimen occurred at a sintering temperature of 800°C. The specimens sintered at temperatures above 800°C had main crystal structure of BaAl₂Si₂O₈.     

Fracture toughness evaluation of WC–10 wt% Co hardmetal sintered under high pressure and high temperature

This work focused on fracture toughness studies of WC–10?wt% Co hardmetal fabricated through the high pressure/high-temperature technique. A powder mixture of WC–10?wt% Co was sintered at 1500–1900°C under a pressure of 7.7?GPa for 2 and 3?min. Vickers hardness test at two different loads of 15 and 30?kgf was done and fracture toughness of the sintered bodies was measured using the indentation method to obtain the effect of sintering parameters. Structural analyses were also performed via X-ray diffraction to investigate structure-related properties. Full density was achieved for high sintering temperature along with abnormal grain growth that reduced hardness. High hardness was observed ranging from 1200 to 1670?HV and fracture toughness increased with increasing sintering temperature up to the highest value of 17.85?MPa/m^1/2.     

Fluoride-doped MWCNT/Si3N4 composite with improved mechanical and structural properties

The addition of carbon nanotubes (CNT) in ceramic composites has stimulated a substantial interest due to their high mechanical, thermal and electrical properties. This approach used fluoride additives (AlF₃ and MgF₂) to prepare multi-walled carbon nanotubes/silicon nitride (MWCNT/Si₃N₄) composite densified at 1700 °C for 1 h by hot press (HP) sintering. The microstructural analyses of MWCNT/Si₃N₄ composites indicate that the fluoride additives have substantially improved densification and the transformation of α-Si₃N₄ to β-Si₃N₄. As observed, the mechanical properties, i.e. flexural strength, fracture toughness, Young's modulus and hardness of MWCNT/Si₃N₄ composites are improved with an increasing concentration of MWCNT. These results attributed to the highly dense composites, strong interfacial interaction and the pull-out mechanism of MWCNT and β-Si₃N₄. The maximum values of fracture toughness flexural strength, Young's modulus, and hardness were 12.76 ± 1.15 MPa.m^0.5, 883 ±46 MPa, 260 ±9 GPa, and 26.4 ± 1.3 GPa, respectively. The improved mechanical properties also ascribed to the synergistic strengthening and toughening influence of MWCNT and β-Si₃N₄.     

Raman studies on nanocomposite silicon carbonitride thin film deposited by r.f. magnetron sputtering at different substrate temperatures

Raman studies of nanocomposite SiCN thin film by sputtering showed that with increase of substrate temperature from room temperature to 500 °C, a transition from mostly sp² graphitic phase to sp³ carbon took place, which was observed from the variation of I_D/I_G ratio and the peak shifts. This process resulted in the growth of C₃N₄ and Si₃N₄ crystallites in the amorphous matrix, which led to increase in hardness (H) and modulus (E) obtained through nanoindentation. However, at a higher temperature of 600 °C, again an increase of sp² C concentration in the film was observed but the H and E values showed a decrease due to increased growth of the graphitic carbon phase. The whole process got reflected in a modified four‐stage Ferrari–Robertson model of Raman spectroscopy. Copyright © 2010 John Wiley & Sons, Ltd.     

Effect of sintering temperature on the elemental diffusion and electrical conductivity of SrTiO<Subscript>3</Subscript>/YSZ composite ceramic

The 50 vol% SrTiO₃/yttria-stabilized zirconia (YSZ) composite ceramic was prepared through powder sintering route in 1400～1500 °C. Only the cubic YSZ and SrTiO₃ phases are detected in all the sintered ceramics, and the typical XRD peak positions of both phases have varied dramatically. The grain sizes and relative densities of all specimens increase evidently with the sintering temperature. The width of the SrTiO₃/YSZ interfacial region increases from 100.4 to 468.8 nm as the sintering temperature rises from 1400 to 1500 °C. The total electrical conductivities of the sample sintered at 1500 °C are remarkably higher than those at 1400 and 1450 °C, while the ion transference numbers drop from 0.837 to 0.731 with sintering temperature from 1400 to 1500 °C. The variations in the electrical properties above can be interpreted based on the effects of sintering temperature on the elemental diffusions during the sintering process.     

High pressure sintering behavior of polycrystalline diamond with tungsten

Polycrystalline diamond was investigated under high pressure and high temperature of 5.0 GPa and 1100–1500 °C in the presence of tungsten. In situ resistance measurements indicated that reactions between diamond and tungsten happened at about 960 °C. Phase analysis demonstrated that WC increased and meta-stability of W₂C decreased clearly at the higher temperature. It is clear from the characterization of the sintered body that the electrical resistance decreased and the density of specimens increased as the sintering temperature rose. The specimen sintered at 1500 °C has a homogeneous microstructure and good conductivity.     

Stabilisation of Ce-Cu-Fe amorphous alloys by addition of Al

The present work describes the formation of amorphous alloys in the (Al_1?xCe_x)₆₂Cu₂₅Fe₁₃ quaternary system (0 ≤ x ≤ 1). When the amount of Ce falls in the range 0.67 ≤ x ≤ 0.83, the alloys obtained exhibit a completely amorphous structure confirmed by powder X-ray diffraction. Otherwise, at compositions x = 0.5, 0.58, 0.92 and 1, a primary crystalline phase forms together with an amorphous matrix. The crystallisation temperature (T_x) decreases with increasing Ce content, varying from 593 K for x = 0.5–383 K for x = 1. Composition x = 0.75 is considered as the best glass former, exhibiting a large supercooled liquid region of 40 K width that precedes crystallisation. In order to form bulk amorphous alloys, ribbons with this later composition were consolidated into few millimetre thick discs using pulsed electric current sintering at different temperatures, yet preserving the amorphous structure. Meanwhile, increasing temperature above 483 K triggers crystallisation of a primary phase isostructural to AlCe₃. Further increase in the temperature up to 573 K yields a higher fraction of the crystalline phase. Testing mechanical properties, using nanoindentation, revealed that both elastic modulus (E) and hardness (H) depend on the Al content, ranging from E = 85.6 ± 3.7 GPa and H = 6.2 ± 0.7 GPa for x = 0.5 down to E = 39.8 ± 1.0 GPa and H = 3.1 ± 0.2 GPa for x = 0.92.