Synthesis and characterization of in situ nanocrystalline intermetallic phase reinforced AlTiSi amorphous matrix composite

Composites with partially amorphous matrix were synthesized by mechanical alloying of an Al₅₀Ti₄₀Si₁₀ elemental powder blend in a high energy planetary ball-mill, followed by high pressure (8 GPa) low temperature (350–450°C) sintering. Microstructural studies and compositional micro-analysis were carried out using scanning and transmission electron microscopy, and energy dispersive spectroscopy, respectively. Phase evolution as a function of milling time and isothermal temperature and their thermal stability was determined by X-ray diffraction at room or elevated temperature and differential scanning calorimetry, respectively. The microstructure of composites sintered between room temperature and 450°C showed nano-size (≈50 nm) crystalline precipitates of Al₃Ti dispersed in an amorphous matrix. The composites sintered at 400°C with 8 GPa pressure exhibited the highest density (3.58 Mg/m³), nanoindentation hardness (8.8 GPa), Young's modulus (158 GPa) and compressive strength (1940 MPa). A lower hardness and modulus on sintering at 450°C is attributed to additional amorphous to nanocrystalline phase transformation and partial coarsening of Al₃Ti.     

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.     

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.     

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.     

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.     

High pressure infiltration sintering behavior of WC-Co alloys

In this paper, two average tungsten carbide particle sizes of 2, 0.5?μm are placed respectively, in contact with a WC-16Co substrate, pressed at the pressure of 4.5–5.5?GPa, and heated to temperatures ranging from 1350°C to 1500°C in a large-volume cubic press. During the process Co was forced out of the WC-16Co substrate into the compressed powder. The resulting infiltrated samples were characterized using X-ray diffraction (XRD), scanning electron microscope (SEM), Vickers hardness and cutting performance tests. The results of XRD confirmed that the sintered bulks have WC and Co phases. The scanning electron microscopy (SEM) analysis reveals that the WC grains in well-sintered alloys are round in shape and cobalt with lower content is uniformly dispersed in the WC grain boundaries. The sintered sub-micron WC-Co alloy with a cobalt content of 3.8?wt% exhibits a prominent combination of high hardness value of 23.1?GPa and a large fracture toughness value of 8.6?MPa?m^½. The high-speed cutting tests indicating its cutting performance is significantly superior to the commercial YG6X (WC-6?wt%Co with WC grain size of 0.5?μm).     

Boron–Carbon Nanocomposites Fabricated at High Pressures and Temperatures

Interaction of amorphous boron and C₆₀ fullerite is analyzed at pressures of 2.0 and 7.7. GPa and temperatures of 600–1800°C. Effect of pressure and temperature on the material structure is studied, temperatures for synthesis of boron carbide and diamond are found, and the sequence of transformations of the carbon component is determined. Ultrasonic method is used to measure elastic moduli of the samples, and the dependences of the moduli on the structure are analyzed. It is demonstrated that the boron–carbon nanocomposite synthesized at relatively low pressure (2.0 GPa) and temperature (about 1000°C) exhibits high elastic parameters (bulk modulus, B ≈ 75.3–84.0 GPa; Young modulus, E ≈ 108–119 GPa; and shear modulus, G ≈ 43–47 GPa at a density of about 2.2 g/cm³). The results can be used for development of novel nanocomposite materials.     

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.     

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.     

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.     

Phase Transitions in a Mixture of Amorphous C<Subscript>60</Subscript> and C<Subscript>70</Subscript> Fullerene Phases at High Temperatures and Pressures

Phase transitions in two types of amorphous fullerene phases (C₆₀–C₇₀ (50/50) mixtures and an amorpous C₇₀ fullerene phase) are studied via neutron diffraction at pressures of 2–8 GPa and temperatures of 200–1100°C. Fullerenes are amorphized by grinding in a ball mill and sintered under quasi-hydrostatic pressure in a toroidal-type chamber. Diffraction studies are performed ex situ. It is shown that the amorphous phase of fullerenes retains its structure at temperatures of 200–500°C, and amorphous graphite is formed at 800–1100°C with a subsequent transition to crystalline graphite. This process is slow in a mixture of fullerenes, compared to C₇₀ fullerene. According to neutron diffraction data, the amorphous graphite formed from amorphous fullerene phases has anisotropy that is much weaker in a fullerene mixture.     

Ti-B-C-N纳米复合薄膜结构及力学性能研究

利用反应磁控溅射方法在单晶硅和高速钢(W18Cr4V)基片上制备出不同C含量Ti-B-C-N纳米复合薄膜. 使用X射线衍射和高分辨透射电子显微镜研究了Ti-B-C-N纳米复合薄膜的组织和微观结构,用纳米压痕仪测试了它们的硬度和弹性模量. 结果表明,利用往真空室通入C₂H₂气体的方法制备得到的Ti-B-C-N纳米复合薄膜中,在所研究成分范围内只发现TiN基的纳米晶. 当C₂H₂流量较小时,C元素的加入可以促进Ti-B-C 关键词： Ti-B-C-N薄膜 磁控溅射 微观结构 力学性能     

The effects of sintering temperatures on dielectric,ferroelectric and electric field-induced strain of lead-free Bi0.5(Na0.78K0.22)0.5TiO3 piezoelectric ceramics synthesized by the sol–gel technique

Lead-free Bi_0.5(Na_0.78K_0.22)_0.5TiO₃ (BNKT) piezoelectric ceramics were synthesized by the sol–gel technique. The effects of sintering temperatures on the crystal structure, microstructure, densification, dielectric, ferroelectric and electric field-induced strain behaviors of the BNKT ceramics were investigated. X-ray diffraction patterns exhibited a pure perovskite structure from 1075 to 1150 °C. A scanning electron microscopy study revealed an increase in grain size with increasing sintering temperature. The density of the ceramics sintered at 1150 °C reaches a maximum value of 5.55 g/cm³, which is 96% of the theoretical density. BNKT ceramics sintered at an optimum temperature of 1150 °C exhibited a high remnant polarization of 18.5 μC/cm², a high electric field-induced strain of 0.20% and dynamic piezoelectric coefficient d₃₃¹ = (S_max/E_max) of 247 pm/V.     

Influence of sintering temperature and pH on the phase transformation,particle size and anti-reflective properties of RHA nano silica powders

Nano silica powders were synthesized from rice husk ash, the most silica-rich raw material, using alkaline extraction followed by acid precipitation. The phase transformation during sintering, the influence of sintering temperature and pH on the particle size and anti-reflective properties of nano silica were investigated. The results showed that the amorphous SiO₂ sintered at 600°C were transformed to a cristobalite structures completely during the sintering process at 800°C and 1100°C. With the increasing sintering temperature and pH, the particle size distributions (d₅₀) were increased respectively in the range of 62–84, 192–240, and 283–329?nm at sintering temperatures of 600°C, 800°C, and 1100°C. When the sintering temperatures were increased at 1100°C, 98.15% and 96.84% of transmittances were obtained respectively at the highest and lowest points of the anti-reflection band and could be used for anti-reflective applications.     

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.     

Effect of high doses of N<Superscript>+</Superscript>, N<Superscript>+</Superscript> + Ni<Superscript>+</Superscript>, and Mo<Superscript>+</Superscript> + W<Superscript>+</Superscript> ions on the physicomechanical properties of TiNi

The surface layer of an equiatomic TiNi alloy, which exhibits the shape memory effect in the martensitic state, is modified with high-dose implantation of 65-keV N⁺ ions (the implantation dose is varied from 10¹⁷ to 10¹⁸ ions/cm²). TiNi samples are implanted by N⁺, Ni⁺-N⁺, and Mo⁺-W⁺ ions at a dose of 10¹⁷–10¹⁸ cm⁻² and studied by Rutherford backscattering, scanning electron microscopy, energy dispersive spectroscopy, X-ray diffraction (glancing geometry), and by measuring the nanohardness and the elastic modulus. A Ni⁺ concentration peak is detected between two maxima in the depth profile of the N⁺ ion concentration. X-ray diffraction (glancing geometry) of TiNi samples implanted by Ni⁺ and N⁺ ions shows the formation of the TiNi (B2), TiN, and Ni₃N phases. In the initial state, the elastic modulus of the samples is E = 56 GPa at a hardness of H = 2.13 ± 0.30 GPa (at a depth of 150 nm). After double implantation by Ni⁺-N⁺ and W⁺-Mo⁺ ions, the hardness of the TiNi samples is ∼2.78 ± 0.95 GPa at a depth of 150 nm and 4.95 ± 2.25 GPa at a depth of 50 nm; the elastic modulus is 59 GPa. Annealing of the samples at 550°C leads to an increase in the hardness to 4.44 ± 1.45 GPa and a sharp increase in the elastic modulus to 236 ± 39 GPa. A correlation between the elemental composition, microstructure, shape memory effect, and mechanical properties of the near-surface layer in TiNi is found.     

Structure-mediated transition in the behavior of elastic and inelastic properties of beach tree bio-carbon

Microstructural characteristics and amplitude dependences of the Young modulus E and of internal friction (logarithmic decrement δ) of bio-carbon matrices prepared from beech tree wood at different carbonization temperatures T _carb ranging from 600 to 1600°C have been studied. The dependences E(T _carb) and δ(T _carb) thus obtained revealed two linear regions of increase of the Young modulus and of decrease of the decrement with increasing carbonization temperature, namely, ΔE ～ AΔT _carb and Δδ ～ BΔT _carb, with A ≈ 13.4 MPa/K and B ≈ ?2.2 × 10^?6 K^?1 for T _carb < 1000°C and A ≈ 2.5 MPa/K and B ≈ ?3.0 × 10^?7 K^?1 for T _carb > 1000°C. The transition observed in the behavior of E(T _carb) and δ(T _carb) at T _carb = 900–1000°C can be assigned to a change of sample microstructure, more specifically, a change in the ratio of the fractions of the amorphous matrix and of the nanocrystalline phase. For T _carb < 1000°C, the elastic properties are governed primarily by the amorphous matrix, whereas for T _carb > 1000°C the nanocrystalline phase plays the dominant part. The structurally induced transition in the behavior of the elastic and microplastic characteristics at a temperature close to 1000°C correlates with the variation of the physical properties, such as electrical conductivity, thermal conductivity, and thermopower, reported in the literature.     

Ba-Zr codoped sodium bismuth titanate by novel alkoxyless wet chemical route: processing and electromechanical behavior

Sodium bismuth titanate (NBT) based ceramics have been shown to be a promising lead-free alternative to commercial piezoelectrics and high capacitance materials. This article reports a novel aqueous citrate gel route for the synthesis of (Na_0.5Bi_0.5)_xBa_1-xTi_yZr_1-yO₃ powders. Instead of alkoxides, usually used in citrate gel route, aqueous citrate solutions of titanium and bismuth were prepared from their respective inorganic salts. These solutions were used to prepare powder of (Na_0.5Bi_0.5)_0.88Ba_0.12Ti_0.96Zr_0.04O₃. The process produced an amorphous xerogel that was readily crystallized to a pseudocubic perovskite phase when calcined at temperatures as low as 500 °C. The decomposition and oxidation of the xerogel was studied using TG-DTA, which showed complete removal of volatile components by 580 °C. The formation of crystalline phases was studied using XRD. SEM was used to evaluate the sintering behavior of the powder. The powder exhibits significant sintering at temperatures 800–900 °C. The polarization behavior of the sintered material was similar to one prepared by conventional solid state route. A maximum polarization of ∼24 μC/cm² and peak bipolar strain ∼0.095% at 44 kV/cm was achieved in the sintered material. PACS 77.22.Ej; 77.84.Dy     

Low-temperature sintering effects on NASICON-structured LiSn<Subscript>2</Subscript>P<Subscript>3</Subscript>O<Subscript>12</Subscript> solid electrolytes prepared via citric acid-assisted sol-gel method

LiSn₂P₃O₁₂ with sodium (Na) super ionic conductor (NASICON)-type rhombohedral structure was successfully obtained at low sintering temperature, 600 °C via citric acid-assisted sol-gel method. However, when the sintering temperature increased to 650 °C, triclinic structure coexisted with the rhombohedral structure as confirmed by X-ray diffraction analysis. Conductivity–temperature dependence of all samples were studied using impedance spectroscopy in the temperature range 30 to 500 °C, and bulk, grain boundary and total conductivity increased as the temperature increased. The highest bulk conductivity found was 3.64?×?10^?5 S/cm at 500 °C for LiSn₂P₃O₁₂ sample sintered at 650 °C, and the lowest bulk activation energy at low temperature was 0.008 eV, showing that sintering temperature affect the conductivity value. The voltage stability window for LiSn₂P₃O₁₂ sample sintered at 600 °C at ambient temperature was up to 4.4 V. These results indicated the suitability of the LiSn₂P₃O₁₂ to be exploiting further for potential applications as solid electrolytes in electrochemical devices.     

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.