Bulk Al-Al3Zr composite prepared by mechanical alloying and hot extrusion for high-temperature applications

Bulk Al/Al₃Zr composite was prepared by a combination of mechanical alloying (MA) and hot extrusion processes. Elemental Al and Zr powders were milled for up to 10 h and heat treated at 600℃ for 1 h to form stable Al₃Zr. The prepared Al₃Zr powder was then mixed with the pure Al powder to produce an Al-Al₃Zr composite. The composite powder was finally consolidated by hot extrusion at 550℃. The mechanical properties of consolidated samples were evaluated by hardness and tension tests at room and elevated temperatures. The results show that annealing of the 10-h-milled powder at 600℃ for 1 h led to the formation of a stable Al₃Zr phase. Differential scanning calorimetry (DSC) results confirmed that the formation of Al₃Zr began with the nucleation of a metastable phase, which subsequently transformed to the stable tetragonal Al₃Zr structure. The tension yield strength of the Al-10wt%Al₃Zr composite was determined to be 103 MPa, which is approximately twice that for pure Al (53 MPa). The yield stress of the Al/Al₃Zr composite at 300℃ is just 10% lower than that at room temperature, which demonstrates the strong potential for the prepared composite to be used in high-temperature structural applications.     

ZrO_2-supported α-MnO_2:Improving low-temperature activity and stability for catalytic oxidation of methane

The single phaseα-Mn O_2and in-situ supportedα-Mn O_2/Zr O_2with different ratios of Mn/Zr were synthesized by one-pot hydrothermal method.They showed superior activity for catalytic oxidation of methane and even better than that of 1%Pt/Al_2O_3.The T_(50)of Mn O_2/Zr O_2catalysts with different ratios of Mn/Zr were located in the range of 315–335°C at a WHSV of 90 L g~(-1)h~(-1),whereas that of Pt/Al_2O_3was 380°C.After sulfur ageing,the Mn O_2/Zr O_2catalysts with Mn/Zr ratio of 2:1(2Mn O_2/1Zr O_2)and 1:1(1Mn O_2/1Zr O_2)exhibited satisfying sulfur resistance in comparison to the pure Mn O_2.The 2Mn O_2/1Zr O_2catalyst also showed acceptable catalytic stability,and the addition of 10 vol%CO_2had no obvious negative effect on its stability,whereas the addition of2.6 vol%H_2O caused slight but reversible decreasing methane oxidative activity.     

Bulk Al–Al3Zr composite prepared by mechanical alloying and hot extrusion for high-temperature applications

Bulk Al/Al3Zr composite was prepared by a combination of mechanical alloying (MA) and hot extrusion processes. Elemental Al and Zr powders were milled for up to 10 h and heat treated at 600°C for 1 h to form stable Al3Zr. The prepared Al3Zr powder was then mixed with the pure Al powder to produce an Al–Al3Zr composite. The composite powder was finally consolidated by hot extrusion at 550°C. The mechanical properties of consolidated samples were evaluated by hardness and tension tests at room and elevated temperatures. The results show that annealing of the 10-h-milled powder at 600°C for 1 h led to the formation of a stable Al3Zr phase. Differential scanning calorime-try (DSC) results confirmed that the formation of Al3Zr began with the nucleation of a metastable phase, which subsequently transformed to the stable tetragonal Al3Zr structure. The tension yield strength of the Al?10wt%Al3Zr composite was determined to be 103 MPa, which is approximately twice that for pure Al (53 MPa). The yield stress of the Al/Al3Zr composite at 300°C is just 10% lower than that at room tem-perature, which demonstrates the strong potential for the prepared composite to be used in high-temperature structural applications.     

Phase transformation and crystal growth behavior of 8mol% (SmO<Subscript>1.5</Subscript>, GdO<Subscript>1.5</Subscript>, and YO<Subscript>1.5</Subscript>) stabilized ZrO<Subscript>2</Subscript> powders

Nanocrystalline powders of ZrO₂-8mol%SmO_1.5(8SmSZ), ZrO₂-8mol%GdO_1.5 (8GdSZ), and ZrO₂-8mol%YO_1.5(8YSZ) were prepared by a simple reverse-coprecipitation technique. Differential thermal analysis/thermogravimetry (DTA/TG), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), Raman spectroscopy, and high-resolution transmission electron microscopy (HRTEM) were used to study the phase transformation and crystal growth behavior. The DTA results showed that the ZrO₂ freeze-dried precipitates crystallized at 529, 465, and 467℃ in the case of 8SmSZ, 8GdSZ, and 8YSZ, respectively. The XRD and Raman results confirmed the presence of tetragonal ZrO₂ when the dried precipitates were calcined in the temperature range from 600 to 1000℃ for 2 h. The crystallite size increased with increasing calcination temperature. The activation energies were calculated as 12.39, 12.45, and 16.59 kJ/mol for 8SmSZ, 8GdSZ, and 8YSZ respectively.     

Effects of homogenization on the dissolution and precipitation behaviors of intermetallic phase for a Zr and Er containing Al-Zn-Mg-Cu alloy

The effects of homogenization on dissolution and precipitation behaviors of intermetallic phase in a novel Zr and Er containing Al-Zn-Mg-Cu alloy were investigated.In this work,single-stage(SS:475℃/24 h) and doublestage(DS:400℃/12 h+475℃/24 h) homogenization treatments were carried out for the ingots with the heating rates of 300℃/h,50℃/h and 25℃/h,respectively.It was found that Er tended to segregate at the grain boundary in the form of Al_8Cu_4Er,and the formation mechanism was determined to be the eutectic reaction in the front of the solid/liquid interface during solidification.Also,Al_8Cu_4Er phase was detected to possess high melting point(～573.8℃),which fully remained after the homogenization.Meanwhile,a significant impact of heating rate on the dissolution of intermetallic phases for the studied alloy under the DS homogenization was determined,but little impact was observed under the SS homogenization.Morever,the size and distribution of the dispersoids after homogenization were fully analyzed.It was found that slow heating rates was helpful to refine the particles size,and increase the density as well as volume fraction of the precipitation under both SS and DS homogenization.However a higher density and volume fraction of the precipitated particles,and a relatively larger average particle size were gained with DS homogenization.     

Preparation and thermal stability of zirconia-doped mullite fibers via sol-gel method

The zirconia-doped mullite fibers were prepared via a sol-gel method from aluminum isopropoxide-aluminum nitrate-tetraethyl orthosilicate system.The effects of zirconia doping on the sol spinnability,mullitization,structure and thermal stability of mullite fibers were investigated by means of Fourier transform infrared(FT-IR) spectroscopy,scanning electron microscopy(SEM) and X-ray diffraction(XRD).The results showed that Zr—O—C bond was presented with the involvement of zirconium acetate,which accelerat...     

Hot deformation behaviors of WE71 alloy under plain strain compression at elevated temperature

Hot deformation behaviors of WE71 (Mg–7Y-1Nd-0.5Zr) alloy was investigated by plain strain compression tests conducted at temperatures ranging from 350 °C to 500 °C and strain rates varying from 0.01 s^-1 to 10 s^-1. Results show that the hot deformation of WE71 was accompanied by the precipitation of rich Zr phase with granular shape and block-shaped phase rich in element Y. When deformed at low temperature and high strain rate, the softening behavior of the alloy was synergically determined by shear bands propagation, adiabatic heating, twinning formation and dynamic recrystallization (DRX). For the conditions of high temperature and high strain rate, DRX was the major softening mechanism while the formation and annihilation of extension twinning resulted in a special flow curve characteristic at the strain of around 0.3. According to the microstructural observations, it can be concluded that the irregular flow curves of WE71 alloy during plain strain compression process are mainly ascribed to shear bands propagation, adiabatic heating, twinning formation and DRX.     

Novel approaches to produce Al2O3– TiC/TiCN– Fecomposite powders directly from ilmenite

Al2O3 –TiC/TiCN–Fe composite powders were successfully prepared directly from ilmenite at 1300–1400℃.The effects of Al/C ratio,sintering atmosphere,and reaction temperature and time on the reaction products were investigated.Results showed that the nitrogen atmosphere was bene cial to the reduction of ilmenite and the formation of Al2O3 –TiC/TiCN–Fe composite powders.When the reaction temperature was between 600 and 1100℃,the intermediate products,TiO2,Ti3O5 and Ti4O7 were found,which changed to TiC or TiCN at higher temperature.Al/C ratio was found to affect the reaction process and synthesis products.When Al addition was 0.5 mol,the Al2O3 phase did not appear.The content of carbon in TiCN rose when the reaction temperature was increased.     

Photocatalytic effect of nature and modified V-bearing rutile

A natural rutile TiO2, which displays photocatalysis on degrading halohydrocarbon pollutants, was reported. The rutile contains up to 1.22% V2O5 (weight percent). Substitutions of Ti by V, as well as Fe, Cu and Zn, result in lattice distortions and defects. Grinding, heating and quenching modify the surface characteristics of ruffle, and consequently increase its photoactivity. It is found that the heating and quenching treatments enhance visible-light absorption of ruffle, especially at 1000 and 1100℃. Ground rutile is effective to degrade tetrachloroethylene and trichloroethylene. While, heating at 1000℃, and quenching at 1000 and 1100℃ distinctly improve degradation rate of samples. The special properties of the natural rutile have particular capabilities in photocatalytic oxidation, especially in degradation of halohydrocarbons.     

Zr-xNb-4Sn alloys with low Young’s modulus and magnetic susceptibility for biomedical implants

The microstructure, mechanical and magnetic properties of Zr–x (8, 9, 10, wt.%)Nb–4Sn alloys were investigated to obtain novel Zr-based alloy with low Young’s modulus and magnetic susceptibility for biomedical implants. After homogenization annealing, hot forging and solution annealing, Zr–8Nb–4Sn, Zr–9Nb–4Sn and Zr–10Nb–4Sn alloys were composed of β+α″ phase, β+α″ phase, β+ω phase, respectively. The temperature at which the α" and ω phase were transformed into β phase during the heating process was about 200 ​°C, and the phase transformation temperature decreased with the increase of Nb element. Among all the Zr–x (x ​= ​8,9,10)Nb–4Sn(wt.%) alloys, Zr–9Nb–4Sn alloy had the lowest Young's modulus of 46.6 ​GPa and the low magnetic susceptibility of 1.294 ​× ​10⁻⁶ cm³g⁻¹, which has a good application prospect for biomedical applications.     

Oxidation behavior of the Fe-36Al-0.09C-0.09B-0.04Zr alloy at 1250°C

To explore and study the Fe-Al system alloy presenting exceptional oxidation resistance at high temperature, the Fe-36Al-0.09C-0.09B-0.04Zr alloy was designed and developed. The microstructure and hardness of the backing at 1250°C were analyzed and measured. Thermodynamics and kinetics of the oxidation behavior were also analyzed by X-ray diffraction, scanning electron microscopy, and energy-dispersive X-ray spectroscopy techniques. The results show that the microstructure of the Fe-36Al-0.09C-0.09B-0.04Zr alloy is FeAl phase at ambient temperature and is stable at 1250°C. It displays the excellent property of oxidation resistance because the oxide film has only the Al₂O₃ layer, and its oxidation kinetics curve obeys the parabolic law at 1250°C. The oxidation mechanism at 1250°C is presumed that in the early oxidation period, the alloy oxidizes to form a large number of Al₂O₃ and a little Fe₂O₃, then, the enrichment of Al caused by Fe oxidization combines with O to form Al₂O₃.     

Improvement of oxidation resistance of Nb–Ti–Si based alloys with additions of Al,Cr and B at different temperatures

The effects of Cr, Al and B addition on the microstructure and high-temperature oxidation behaviors (at 1200, 1250 and 1300 ?°C) of Nb–Ti–Si based alloys were investigated. The results showed that the addition of Cr stabilized α-Nb₅Si₃, while Al promoted the formation of β-Nb₅Si₃ and adding B promoted the formation of γ-Nb₅Si₃. Among the three elements, Al and Cr were beneficial to oxidation resistance at 1200 ?°C, and B was favorable to the oxidation resistance at 1300 ?°C. At 1250 ?°C, Al and B had the same effects on the improvement of oxidation resistance. The ratio of these alloying elements might play an important role in enhancing oxidation resistance. The oxidation resistance of the three kinds of silicides was compared, and the sequence was: γ-Nb₅Si₃> β-Nb₅Si₃> α-Nb₅Si₃. To predict the effects of the investigated alloying elements on the oxidation resistance of Nb–Ti–Si based alloys in a wider range of concentration, an artificial neural network (ANN) model was established, showing excellent accuracy and generalization ability. With the instructions of the ANN model, the oxidation resistance can be optimized with less additions of alloying elements.     

Effect of temperature and stress on high temperature creep behavior of Ni3Al-based single crystal superalloy

The creep behavior and dislocations mechanism of the Ni₃Al-based single crystal alloy IC6SX with [001] orientation were investigated under the testing conditions of 1100 ?°C/137 ?MPa, 1100 ?°C/120 ?MPa and 1070 ?°C/137 ?MPa. It was observed that the temperature and stress had a significant effect on the high temperature creep life of the single crystal alloy. As the temperature was reduced from 1100 ?°C to 1070 ?°C, the creep life increased from 65.07 ?h to 313.8 ?h. As the stress was reduced to 120 ?MPa, the creep life increased to 243.3 ?h. Under the high temperature and low stress condition the dislocations entered the γ′ phase by climbing caused by the atomic diffusion, instead of slipping.     

Microstructure and oxidation behavior of carbon fiber reinforced SiC composite (Cf/SiC) with Mo–57Si–10B oxidation protection coating

Mo–57Si–10B (at.%) coating was prepared by the spark plasma sintering (SPS) technique on a 2D woven C_f/SiC composite, and the oxidation behavior of the bare and the coated C_f/SiC samples at 1300 ?°C were investigated. The coating was composed of a fine MoSi₂/MoB/SiO₂/Mo₂B₅ out layer and the inner SiO₂ interface layer. The mass gain percentage was approximately 0.25% after oxidation at 1300 ?°C for 100 ?h. The coated C_f/SiC substrate was effectively protected, owing to the rapid formation of the dense and protective borosilicate layer on the coating, the excellent microstructure stability of the coating and the inner SiO₂ interface layer.     

A TEM study on the microstructure of spark plasma sintered ZrB_2-based composite with nano-sized SiC dopant

Sintering behavior of ZrB_2 ceramic with nano-sized SiC dopant was studied. ZrB_2-25 vol% nano-sized SiC was selected as the starting mixture to fabricate the composite. The manufacturing process was accomplished at 1800℃ for 5 min under 25 MPa via spark plasma sintering(SPS). The as-sintered sample reached a relative density of 99%. Besides the initial phases, namely ZrB_2 and SiC, the high-resolution X-ray diffraction(HRXRD) was used to study the formation of an in-situ ZrC phase. The possible chemical interactions during the ZrC phase formation were scrutinized. The microstructure of the composite was studied by the field emission scanning electron microscopy(FESEM) and transmission electron microscopy(TEM). Elemental analysis through FESEM evaluations revealed the formation of amorphous phases, rich in Zr, C, Si, B, and O elements, which was in harmony with the thermodynamical assessments. TEM studies endorsed the formation of such phases, containing a glassy bed of Si–B–O with ZrC and C islands dispersed therein.     

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.     

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.     

Carbothermal synthesis of Si3N4 powders using a combustion synthesis precursor

Si₃N₄ powders were synthesized by a carbothermal reduction method using a SiO₂ + C combustion synthesis precursor derived from a mixed solution consisting of silicic acid (Si source), polyacrylamide (additive), nitric acid (oxidizer), urea (fuel), and glucose (C source). Scanning electron microscopy (SEM) micrographs showed that the obtained precursor exhibited a uniform mixture of SiO₂ + C composed of porous blocky particles up to ～20 μm. The precursor was subsequently calcined under nitrogen at 1200–1550°C for 2 h. X-ray diffraction (XRD) analysis revealed that the initial reduction reaction started at about 1300°C, and the complete transition of SiO₂ into Si₃N₄ was found at 1550°C. The Si₃N₄ powders, synthesized at 1550°C, exhibit a mixture phase of α- and β-Si₃N₄ and consist of mainly agglomerates of fine particles of 100–300 nm, needle-like crystals and whiskers with a diameter of about 100 nm and a length up to several micrometers, and a minor amount of irregular-shaped growths.     

Microstructure and mechanical properties of spark plasma sintered Ti-Mo alloys for dental applications

Ti-Mo alloys with various Mo contents from 6wt% to 14wt% were processed by spark plasma sintering based on elemental powders. The influence of sintering temperature and Mo content on the microstructure and mechanical properties of the resulting alloys were investigated. For each Mo concentration, the optimum sintering temperature was determined, resulting in a fully dense and uniform microstructure of the alloy. The optimized sintering temperature gradually increases in the range of 1100–1300℃ with the increase in Mo content. The microstructure of the Ti-(6–12)Mo alloy consists of acicular α phase surrounded by equiaxed grains of β phase, while the Ti-14Mo alloy only contains single β phase. A small amount of fine α lath precipitated from β phase contributes to the improvement in strength and hardness of the alloys. Under the sintering condition at 1250℃, the Ti-12Mo alloy is found to possess superior mechanical properties with the Vickers hardness of Hv 472, the compressive yield strength of 2182 MPa, the compression rate of 32.7%, and the elastic modulus of 72.1 GPa. These results demonstrate that Ti-Mo alloys fabricated via spark plasma sintering are indeed a perspective candidate alloy for dental applications.     

Synthesis of nano onion-like fullerenes by using Fe/Al2O3 as catalyst by chemical vapor deposition

Nano-carbon materials were synthesized by the catalytic decomposition of acetylene at 400℃ by using Fe/Al₂O₃ as catalyst. The product was refluxed in 36% concentrated HCl at 60℃ for 48 h in order to remove the catalyst support. The samples were examined by scanning and high resolution transmission electron microscopy, energy dispersive spectroscopy and X-ray diffraction. The results show that nano onion-like fullerenes encapsulating a Fe₃C core were obtained. These had a structure of stacked graphitic fragments, with diameters ranging from 15―50 nm. When the product was further heat- treated at 1100℃ for 2 h, nano onion-like fullerenes with a clear concentric graphitic layer structure were obtained. The growth mechanism of nano onion-like fullerenes encapsulating metal cores is suggested to follow a vapor-solid growth model.