Effect of sintering temperature on the preparation of Cu–Ti3SiC2 metal matrix composite

Ti3SiC2 has the potential to replace graphite as reinforcing particles in Cu matrix composites for applications in brush,electrical contacts and electrode materials.In this paper the fabrication of Cu-Ti3SiC2 metal matrix composites prepared by warm compaction powder metallurgy forming and spark plasma sintering(SPS) was studied.The stability of Ti3SiC2 at different sintering temperatures was also studied.The present experimental results indicate that the reinforcing particles in Cu-Ti3SiC2 composites are not stable at and above 800℃.The decomposition of Ti3SiC2 will lead to the formation of TiC and/or other carbides and TiSi2.If purity is the major concern,the processing and servicing temperatures of the Cu-Ti3SiC2 composite should be limited to 750℃ or lower.The composites prepared by warm compaction forming and SPS sintering at 750℃ have lower density when compared with the composites prepared by SPS sintering at 950℃,but their electrical resistivity values are very close to each other and even lower.     

Rapid reactive synthesis of TiAl3 intermetallics by thermal explosion and its oxidation resistance at high temperature

Porous TiAl₃ intermetallics were synthesized from Ti-75 at.% Al elemental powder mixtures using an energy-saving and rapid reactive method of thermal explosion (TE). The results demonstrated that the actual temperature of the compact climbed rapidly from 673 °C to 1036 °C within 24 s, indicating that an obvious TE reaction occurred during sintering process. The video graphs suggested that the TE in Ti–Al system behaved instant occurrence and overall heating whether from axial or radial direction. The silver wires and NaCl particles that pressed on the surface of the sample disappeared due to the heavy heat released during TE reaction. Only pure TiAl₃ phases were synthesized in TE products and the open porosity of 55.4% was easy to obtain. After high-temperature treatment at 1000 °C, large amounts of sintering-neck formed and then improved the compressive strength of porous TiAl₃ materials. Moreover, the mass gain curve of porous TiAl₃ intermetallics oxidized at 650 °C for 120 h exhibited the parabolic oxidation rate law. XPS analysis confirmed that the strong O 1s peak was 531.4 eV which was the typical binding energy of Al₂O₃. Therefore, the excellent oxidation resistance of porous TiAl₃ foams would be considered as good candidate materials for prolonging the service life at high temperatures.     

Effect of sintering temperature on phase evolution of Al_(86)Ni_6Y_(4.5)Co_2La_(1.5) bulk amorphous composites synthesized via mechanical alloying and spark plasma sintering

Al_(86)Ni_6Y_(4.5)Co_2La_(1.5) amorphous powders were synthesized by mechanical alloying for 200 h. Subsequent consolidation was performed via spark plasma sintering in the temperature range of 250 ℃ to 500 ℃ at the pressure of 500 MPa. The role of viscous flow on densification was investigated by studying the viscosity change of the amorphous phase at different consolidation temperatures. The decrease in viscosity at higher sintering temperatures resulted in better particle bonding and densification of consolidated samples. The formation of only FCC Al was observed in the consolidated samples at sintering temperatures ≤ 300 ℃ and the intermetallic phases formed at temperatures ≥ 400 ℃. The mechanical properties of the bulk samples were measured by Vickers microhardness and nanoindentation tests. The testing results showed that the average values of microhardness, nanohardness and elastic modulus of the sample consolidated at 500 ℃ were 3.06 ± 0.14 GPa,4.85 ± 1.14 GPa and 89.53 ± 9.25 GPa, respectively. The increase in hardness and elastic modulus of the higher temperature consolidated samples is attributed to the improvement in particle bonding, densification and distribution of various hard intermetallic phases in the amorphous matrix.     

Effects of annealing temperature on the microstructure and hardness of TiAlSiN hard coatings

TiAlSiN hard coatings were synthesized on high-speed steel using an arc ion enhanced magnetic sputtering hybrid system.The microstructure and hardness of the coatings at different annealing temperatures were explored by means of XRD,TEM,EDAX and Vickers indentation.The as-deposited TiAlSiN coatings were confirmed to be amorphous due to high depositing rate and low deposition temperature during the film growth.The transformation from amorphous to nanocomposites of nano-crystallites and amorphousness were observed after the annealing treatment,the microstructure of TiAlSiN coatings annealed at 800°C and 1000°C were consisted of crystalline hcp-AlN,fcc-TiN and amorphous phase,however,the coatings were only consisted of fcc-TiN and amorphous phase when annealing at 1100°C and 1200°C.Meanwhile,the formation of Al2O3 was detected on the coating surface after annealing at 1200°C and it indicated the excellent oxidation resistance of the TiAlSiN coatings under the present experimental conditions.Furthermore,the average grain size of the TiAlSiN coatings after high temperature annealing even at 1200°C was less than 30 nm and the size increased with the increasing temperature.However,the hardness of the so-deposited coatings with HV0.2N=3300 dramatically decreased with the increase of temperature and reached nearly to the hardness of TiN coatings with HV0.2N=2300.     

Sintering mechanism of Cu-9Al alloy prepared from elemental powders

The sintering behavior of Cu-9Al alloys prepared from die pressing of elemental powders was investigated. The experimental results and kinetic analysis showed the formation of three consecutive layers of Al₂Cu, Al₄Cu₉, and AlCu phases, with Al₂Cu appearing first in the initial solid phase sintering stage. A liquid phase formed in the intermediate stage, resulting from the eutectic reaction between Al and Al₂Cu phases at 500 °C, which is 47 °C lower than the equilibrium reaction temperature. Swelling occurred when the liquid phase infiltrated the gaps between the copper particles, leaving pores at the original sites of Al particles and Al₂Cu. In the final stage of sintering, the Al-rich phases (Al₂Cu and AlCu) transformed to Al-poor phases (Al₄Cu₉ and α-Cu) in the temperature range of 500–565 °C. Al₄Cu₉ and α-Cu then transformed to AlCu₃ (β) above the eutectoid reaction temperature (565 °C), whereas AlCu₃ transformed to α-Cu and eutectoid phases (α-Cu + Al₄Cu₉) during cooling. The pure copper transformed to AlCu₃, and the pore volume decreased at 1000 °C. The microstructure study helps manipulate precisely the sintering process of Cu-Al alloys and optimize the microstructure with a high dimensional accuracy.     

High-temperature mechanical properties and deformation behavior of high Nb containing TiAl alloys fabricated by spark plasma sintering

A high Nb containing TiAl alloy was prepared from the pre-alloyed powder of Ti-45Al-8.5Nb-0.2B-0.2W-0.02Y (at%) by spark plasma sintering (SPS). Its high-temperature mechanical properties and compressive deformation behavior were investigated in a temperature range of 700 to 1050℃ and a strain rate range of 0.002 to 0.2 s-1. The results show that the high-temperature mechanical properties of the high Nb containing TiAl alloy are sensitive to deformation temperature and strain rate, and the sensitivity to strain rate tends to rise with the deformation temperature increasing. The hot workability of the alloy is good at temperatures higher than 900℃, while fracture occurs at lower temperatures. The flow curves of the samples compressed at or above 900℃ exhibit obvious flow softening after the peak stress. Under the deformation condition of 900-1050℃ and 0.002-0.2 s-1, the interrelations of peak flow stress, strain rate, and deformation temperature follow the Arrhenius' equation modified by a hyperbolic sine function with a stress exponent of 5.99 and an apparent activation energy of 441.2 kJ·mol-1.     

Synthesis and characterization of Cr2AlC with nanolaminated particles

In this work, we reported the large-scale and low cost synthesis of high purity Cr2 AlC powders with nanolaminated particles by pressureless sintering. The chemical reactions involved in synthesizing Cr2 AlC had been studied and discussed. The results showed that the Al contents in the starting materials and sintering temperatures had significant effects on the synthesis and purity of Cr2 AlC. The obtained high purity Cr2 AlC powders were stable up to at least 1400 °C. The Cr2 AlC powders consisted of nanolaminated particles, the size of which was tunable by adjusting sintering time. The present synthesized nanolaminated Cr2 AlC powders would be an excellent reinforcement material for metal matrix composites.     

Improving the tensile properties of extruded Mg–Ga alloy by ageing treatment

A hot-extruded Mg-5Ga alloy was subjected to ageing treatment at 150 ?°C, 190 ?°C and 230 ?°C. The microstructures and mechanical properties of the extruded and aged alloy were examined in this study. Microstructure examinations suggested that particle-shaped and rod-shaped Mg₅Ga₂ were precipitated in the alloy after peak ageing treatment. The extruded alloy showed the yield strength, ultimate tensile strength and elongation to fracture of 157.6 ?MPa, 248.6 ?MPa and 17.5%, respectively. After peak ageing, the yield strength and ultimate tensile strength can be enhanced by as much as 15.7% and 8.6% reaching 182.3 ?MPa and 270 ?MPa, respectively. The improvement of the tensile strengths is mainly attributed to the enhanced precipitation strengthening by newly formed fine Mg₅Ga₂ precipitates. The ductility of the alloy was slightly increased by peak ageing at low temperatures (150 ?°C and 190 ?°C), but remarkably decreased by peak ageing at high temperature (230 ?°C) due to the formation of coarsened Mg₅Ga₂ particles which easily initiated the cracks during tensile deformation.     

Synthesis of glass ceramics from kaolin and dolomite mixture

Cordierite-and anorthite-based binary glass ceramics of the CaO-MgO-Al₂O₃-SiO₂ (CMAS) system were synthesized by mixing local and abundant raw minerals (kaolin and doloma by mass ratio of 82/18). A kinetics study reveals that the activation energy of crystallization (Ea) calculated by the methods of Kissinger and Marotta are 438 kJ·mol-1 and 459 kJ·mol-1, respectively. The Avrami parameter (n) is estimated to be approximately equal to 1, corresponding to the surface crystallization mechanism. X-ray diffraction (XRD) analysis shows that the anorthite and cordierite crystals are precipitated from the parent glass as major phases. Anorthite crystals first form at 850℃, whereas the μ-cordierite phase appears after heat treatment at 950℃. Thereafter, the cordierite allotropically transforms to α-cordierite at 1000℃. Complete densification is achieved at 950℃; however, the density slightly decreases at higher temperatures, reaching a stable value of 2.63 kg·m-3 between 1000℃ and 1100℃. The highest Vickers hardness of 6 GPa is also obtained at 950℃. However, a substantial decrease in hardness is recorded at 1000℃; at higher sintering temperatures, it slightly increases with increasing temperature as the α-cordierite crystallizes.     

Preparation and characterization of CoFe2O4/SiO2 nanocomposites

Recent years see an increasing interest in nanocomposites synthesized by a sol-gel procedure consisting of magnetic nanosized particles embedded in a silica matrix. due to their specific physical and chemical properties[1―4]. Sol-gel derived amorphous si…     

Synthesis and performance of Ca-α/β-SiAlON composites from tailings

Ca-α/β-SiAlON composites were prepared using Ca-α/β-SiAlON powder synthesized from gold ore tailings, which contained abundant Si and Al elements as the major raw materials together with minor additives, through a pressure-less sintering method. The influences of sintering temperature on the phase composition and microstructure of the composites were analyzed. The scanning electron microscopy images of the composites show the interlacing of grains with elongated columnar, short columnar and plate-like morphologies. The composites sintered at 1520℃ for 6 h have a flexural strength of 352 MPa, Vickers hardness of 11.2 GPa, and fracture toughness of 4.8 MPa·m1/2. The relative content of each phase in the products is I(Ca-α-SiAlON):I(β-SiAlON):I(Fe₃Si) = 23:74:3, where I_i stands for the diffraction peak intensity of phase i.     

Extraction of vanadium from high calcium vanadium slag using direct roasting and soda leaching

The extraction of vanadium from high calcium vanadium slag was attempted by direct roasting and soda leaching. The oxidation process of the vanadium slag at different temperatures was investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), and energy dispersive spectroscopy (EDS). The effects of roasting temperature, roasting time, Na₂CO₃ concentration, leaching temperature, leaching time, and liquid to solid ratio on the extraction of vanadium were studied. The results showed that olivine phases and spinel phases in the vanadium slag were completely decomposed at 500 and 800℃, respectively. Vanadium-rich phases were formed at above 850℃. The leaching rate of vanadium reached above 90% under the optimum conditions:roasting temperature of 850℃, roasting time of 60 min, Na₂CO₃ concentration of 160 g/L, leaching temperature of 95℃, leaching time of 150 min, and liquid to solid ratio of 10:1 mL/g. The main impurities were Si and P in the leach liquor.     

Photoluminescence from Ge-SiO2 thin films and its mechanism

Ge-SiO₂ thin films were deposited on p-type Si substrates using the radio frequency (rf) magnetron sputtering technique with a Ge-SiO₂ composite target. Films were annealed in N₂ ambience for 30 min at 300℃—1000℃ with an interval of 100℃. Through the X-ray diffraction, the average size of Ge nanocrystals (nc-Ge) was determined. They increased from 3.9 to 6.1 nm with increasing annealing temperature in the range of 600℃—1000℃. Under ultraviolet excitation, all samples emit a strong violet band centered at 396 nm. With the formation of nc-Ge, the samples exhibit another emission of orange band with the peak at 580 nm and its intensity increases with the increasing size of nc-Ge. The peak positions of two bands do not shift obviously. Experimental data indicate that the violet band comes from GeO defect and the orange band originates mainly from the luminescence centers at the interface between the nc-Ge and SiO₂ matrix.     

Synthesis and characterization of a three-ring bent-core compound

To investigate the vacuum-deposited films of the banana-shaped mesogens, we prepared a three-ring bent-core （that is, banana-shaped） compound m-bis（4-p-octoxysryrenyl）benzene （m-OSB） and used it as a prototype for studying the related film physics. Herein the synthesis and the structural characterization of m-OSB are reported.^13C and ^1H NMR spectra and ^1R spectrum confirm that m-OSB has a symmetric and all-trans conformation. The results of differential scanning calorimetry, polarizing optical microscopy and X-ray diffractometry indicate that no liquid crystalline phase but two crystalline phases are present in this material： phase Ⅰ （T〈66℃） and phase Ⅱ （66~C〈T〈157℃）; an isotropic state is observed at above 157℃. Combining the X-ray diffraction and the electronic diffraction, we assign the room-temperature crystalline phase I to orthorhombie system and P212121 space group with cell parameters of a = 7.43A°. b=6.34A°, c=72.07A°, and α=β=γ=90°. Molecular modeling reveals that the molecules in the unit cell adopt a layered structure with an antiferro-eleetrie alignment. The structure of phase Ⅱ is very similar to that of phase Ⅰ. Nonlinear optical measurement shows that m-OSB is active for the second harmonic generation （SHG）. Such characterization of the bulk material is necessary for the understanding of the growth and microstructures in the films.     

Optimum sintering conditions for optical properties of translucent aluminum nitride ceramics

High translucency is one of the excellent properties of AlN ceramics because of its wide optical band gap energy of 6.2 eV. We have achieved success in producing AlN ceramic tube of 98% total visible light transmittance at 0.6 mm thick tube wall by applying an improved sintering technique. This AlN ceramic was produced by sintering at 1880℃ using Ca3Al2O6 as a sintering additive and in reduction atmosphere to remove the sintering additive from the final sintered material. After the sintering, the annealing ...     

Dielectric anomalies in CaCu3Ti4O12 at high temperatures

We reported the dielectric properties of CaCu3Ti4O12 in the temperature range from room temperature to 800℃ and the frequency range from 20 Hz to 10 MHz.Apart from the widely reported dielectric anomaly occurring around 200℃,three additional dielectric anomalies were found.The new anomalies are very sensitive to electrode sintering conditions and annealing atmospheres,indicating that they are dependent not only on the electrode-sample contact but also on oxygen vacancies.     

Studies on the effects of pre-firing and sintering temperature on NSDC nanocomposite electrolytes

Solid oxide fuel cells (SOFCs) technology, with fuel flexibility, is one of the most promising power generation technology. However, the high operating temperature of SOFCs has hindered their commercial applications. As a crucial requirement to enhance its performance, SOFCs electrolytes should operate at a low temperature. Carbonate/ceria composites are developed as electrolytes for low operating temperature SOFCs, and a better understanding of the mechanism of its ionic conductivity serves this purpose. In this work, ceria-carbonate composite electrolyte, Na₂CO₃/samarium doped ceria (NSDC) were synthesized by the co-precipitation method. The synthesized electrolytes were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), and UV–Vis spectroscopy. The XRD and SEM results showed that the sintered NSDC nanocomposite comprised a single-phase dense electrolyte structure. The crystallite size of the NSDC nanocomposite was greatly affected by the different pre-firing temperatures and different sintering temperatures. Also, the ionic conductivity of the prepared NSDC nanocomposite electrolytes was strongly dependent on the pre-firing and sintering temperatures. The NSDC nanocomposite electrolytes were pre-fired at 950 ?°C and 650 ?°C and sintered at 1200 ?°C and 900 ?°C respectively, had ionic conductivity in H₂ and air high as 0.36 ?S/cm and 0.3 ?S/cm.     

Blue light emission of porous silicon subjected to RTP treatments

Porous silicon samples were treated with the rapid thermal process (RTP) under different circumstances (N2, Ar, O2 and Air). Before and after treatments, the samples were checked by means of photoluminescence (PL) spectroscopy and Fourier transform infrared spectroscopy (FTIR). Four blue light emission peaks were found in the PL spectra of porous silicon samples subjected to the RTP treatments at temperatures above 400℃. The peak positions were found not to vary with the circumstances and temperatures of RTP treatments. It is considered that due to oxidation during the RTP treatments, the pole size of Si crystal in porous silicon decreased, resulting in the blue shift of light emission. Correlated with the Si crystal sizes discontinuous hypothesis and previous researchers' theory calculation, the PL peak positions did not vary with the RTP temperature and circumstances.     

Dispersion of CoCl2 into γ-Al2O3 studied by positron

Co²⁺/γ-Al₂O₃ samples were prepared by incipient wetness impregnation of γ-Al₂O₃ with different concentration solution of CoCl₂ and dried at 40 °C. We measured the positron lifetime spectra of the samples of different Co²⁺ mass fractions (0%–8.24%) heated at different temperatures (100–500°C). All lifetime spectra were resolved into four components, in which the third and the fourth components were related to the surface state of the micropores and the secondary pores of the γ-Al₂O₃. The experimental results showed that the Co²⁺ was mainly located in the micropores and the secondary pores near to the exterior of the support. For low Co²⁺ mass fraction samples, when the heating temperature was above 400 °C, dispersal was almost finished. When the Co²⁺ mass fraction was above 5.59%, Co²⁺ and Cl⁻ were dispersed into the secondary pores in the form of multiple layers.     

The formation and stability of Si1-x C x alloys in Si implanted with carbon ions

Si_1-xC_x alloys of carbon (C) concentration between 0.6%—1.0% were grown in Si by ion implantation and high temperature annealing. The formation of Si_1-xC_x alloys under different ion doses and their stability during annealing were studied. If the implanted dose was less than that for amorphizing Si crystals, the implanted C atoms would like to combine with defects produced during implantation and it was difficult to form Si_1-xC_x alloys after being annealed at 850℃. With the increment of implanted C ion doses, the lattice damage increased and it was easier to form Si_1-xC_x alloys. But the lattice strain would become saturate and only part of implanted carbon atoms would occupy the substitutional positions to form Si_1-xC_x alloys as the implanted carbon dose increased to a certain degree. Once Si_1-xC_x alloys were formed, they were stable at 950℃, but part of their strain would release as the annealing temperature increased to 1 000℃. Stability of the alloys became worse with the increment of carbon concentration in the alloys.