Microstructure,thermal properties,and corrosion behaviors of FeSiBAlNi alloy fabricated by mechanical alloying and spark plasma sintering

An equiatomic FeSiBAlNi amorphous high-entropy alloy (HEA) was fabricated by mechanical alloying (MA). A fully amorphous phase was obtained in the FeSiBAlNi HEA after 240 h of MA. The bulk FeSiBAlNi samples were sintered by spark plasma sintering (SPS) at 520 and 1080℃ under a pressure of 80 MPa. The sample sintered at 520℃ exhibited an amorphous composite structure comprising solid-solution phases (body-centered cubic (bcc) and face-centered cubic (fcc) phases). When the as-milled amorphous HEA was consolidated at 1080℃, another fcc phase appeared and the amorphous phase disappeared. The sample sintered by SPS at 1080℃ exhibited a slightly higher melting temperature compared with those of the as-milled alloy and the bulk sample sintered at 520℃. The corrosion behaviors of the as-sintered samples were investigated by potentiodynamic polarization measurements and immersion tests in seawater solution. The results showed that the HEA obtained by SPS at 1080℃ exhibited better corrosion resistance than that obtained by SPS at 520℃.     

Synthesis and sintering of beryllium oxide nanoparticles

BeO nanoparticles were prepared by polyacrylamide gel route and the sintering pr operties of synthesized powder as a function of sintering temperature and time were investigated. Thermal behaviors of the polyacrylamide gel and beryllium salt we re studied by thermogravimetry analysis (TGA). The calcination temperature (690°C) of the beryllium sulfate covered in polyacrylamide xerogel was almost 150 °C lower than that obtained by traditional methods. The nanocrystallites of the BeO particles were estimated by X-ray diffraction (X RD) according to Debye–Scherrer equation. Transmission electron microscopy (TEM) investigation revealed that the average part icle size of the BeO nanoparticles prepared by calcining at 800 °C for 2 h, ranges from 15 nm to 25 nm. The sintering temperature was down to 1 600 °C, which was around 200 °C lower than conventional sintering temperature of the compact sample with co mmon powders. The densification rate was fast at the first 3 h. The thermal conductivity of the sample sintered at 1 600 °C for 6 h was 186.6 W/(m·K).     

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.     

Spark plasma and microwave sintering of Al6061 and Al2124 alloys

Despite the importance of aluminum alloys as candidate materials for applications in aerospace and automotive industries, very little work has been published on spark plasma and microwave processing of aluminum alloys. In the present work, the possibility was explored to process Al2124 and Al6061 alloys by spark plasma and microwave sintering techniques, and the microstructures and properties were compared. The alloys were sintered for 20 min at 400, 450, and 500℃. It is found that compared to microwave sintering, spark plasma sintering is an effective way to obtain homogenous, dense, and hard alloys. Fully dense (100%) Al6061 and Al2124 alloys were obtained by spark plasma sintering for 20 min at 450 and 500℃, respectively. Maximum relative densities were achieved for Al6061 (92.52%) and Al2124 (93.52%) alloys by microwave sintering at 500℃ for 20 min. The Vickers microhardness of spark plasma sintered samples increases with the increase of sintering temperature from 400 to 500℃, and reaches the values of Hv 70.16 and Hv 117.10 for Al6061 and Al2124 alloys, respectively. For microwave sintered samples, the microhardness increases with the increase of sintering temperature from 400 to 450℃, and then decreases with the further increase of sintering temperature to 500℃.     

Thermoelectric properties of BiSbx (x=0.6-0.8) thermoelectric materials fabricated by different processing

In order to improve the thermoelectric properties, hot-pressing sintering and ultra high pressure sintering methods were adopted to fabricate BiSb_x. The phase and crystal structures were determined by X-ray diffraction analysis (XRD). The thermoelectric properties were measured at 303 K along the direction parallel to the pressing direction. The electric conductivity of the samples was measured at 303 K by the four-probe technique. To measure the Seebeck coefficient, heat was applied to the samples placed between two Cu discs. The thermoelectric electromotive force (E) was measured upon applying small temperature differences ( △T<2℃) between the both ends of the samples. The Seebeck coefficient of the samples was determined from the value of E/△T. The results indicate that the thermoelectric properties of the samples fabricated by UHPS (ultra high pressure sintering) method are much higher than that by HPS (hot pressing sintering) method and have the highest values at x=0.7.     

Effect of CuO addition on the sintering temperature and microwave dielectric properties of CaSiO3– Al2O3 ceramics

CuO-doped CaSiO3–1 wt% Al2O3 ceramics were synthesized via a traditional solid-state reaction method, and their sintering behavior,microstructure and microwave dielectric properties were investigated. The results showed that appropriate CuO addition could accelerate the sintering process and assist the densification of CaSiO3–1 wt% Al2O3 ceramics, which could effectively lower the densification temperature from1250 1C to 1050 1C. However, the addition of CuO undermined the microwave dielectric properties. The optimal amount of CuO addition was found to be 0.8 wt%, and the derived CaSiO3–Al2O3ceramic sintered at 1100 1C presented good microwave dielectric properties of εr?7.27,Q f?16,850 GHz and τf? 39.53 ppm/1C, which is much better than those of pure CaSiO3 ceramic sintered at 1340oC(Q f?13,109 GHz).The chemical compatibility of the above ceramic with 30 Pd/70 Ag during the cofiring process has also been investigated, and the result showed that there was no chemical reaction between palladium–silver alloys and ceramics.& 2014 Chinese Materials Research Society. Production and hosting by Elsevier B.V. All rights reserved.     

Novel trichromatic phosphor Co-doped with Eu, Tb in SiO2 gel matrix

The Eu, Tb co-doped SiO2 matrix tricolor fluorescence system was prepared by sol-gel technique. Red emission at 618 nm, green emission at 543 nm and blue emission at 350-500 nm were observed in the PL spectra of the sample, indicating that Eu^3＋, Eu^2＋ and Tb^3＋ ions coexisted in the matrix. In the co-doped sample, the blue emission of Eu^2＋ was much stronger than that of the sample single doped with Eu, which implied that the electron transfer between Eu^3＋ and Tb^3＋ maybe happened in the SiO2 matrix. The influences of the annealing temperature and Tb concentration on the PL spectra of the samples were investigated. The optimal doped concentration of Tb was determined to be 0.2% and the optimal annealing temperature 850℃. Annealed at 600℃, Tb^3＋ had a sensitizing effect on Eu^3＋ in the SiO2 matrix, and the emission intensity of Eu^3＋ in the Eu, Tb co-doped sample was more than four times that of the single doped sample, which could be attributed to the energy transfer from Tb^3＋ to Eu^3＋.     

Effect of high pressure sintering and annealing on microstructure and thermoelectric properties of nanocrystalline Bi2Te2.7Se0.3 doped with Gd

Bi2Te2.7Se0.3of high performance doped with Gd bulk materials was prepared by a high pressure(6.0 GPa) sintering(HPS) method at 593 K,633 K, 673 K and 693 K. The sample was then annealed for 36 h in a vacuum at 633 K. The phase composition, crystal structure and morphology of the sample were analyzed by X-ray diffraction and scanning electron microscopy. The electric conductivity, Seebeck coefficient, and thermal conductivity aspects of the sample were measured from 298 K to 473 K. The results show that high pressure sintering and the doping with Gd has a great effect on the crystal structure and the thermoelectric properties of the samples. The samples are consisted of nanoparticles before and after annealing, and these nanostructures have good stability at high temperature. HPS together with annealing can improve the TE properties of the sample by decreasing the thermal conductivity of the sample with nanostructures. The maximum ZT value of 0.74 was obtained at 423 K for the sample, which was sintered at 673 K and then annealed at 633 K for 36 h. Compared with the zone melting sample, it was increased by 85% at423 K. Hence the temperature of the maximum of figure of merit was increased. The results can be applied to the field of thermoelectric power generation materials.     

Microwave assisted synthesis &; properties of nano HA-TCP biphasic calcium phosphate

Biphasic calcium phosphate (BCP) nanopowders were synthesized by using microwave and non-microwave irradiation assisted processes. The synthesized powders were pressed under a pressure of 90 MPa, and then were sintered at 1000-1200℃ for 1 h. The mechanical properties of the samples were investigated. The formed phases and microstructures were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The results showed that the synthesis time was shorter, along with a more homogeneous microstructure, when the microwave irradiation assisted method was applied. The compression strength and the Young's modulus of the samples synthesized with microwave irradiation were about 60 MPa and 3 GPa, but those of the samples synthesized without microwave irradiation were about 30 MPa and 2 GPa, respectively. XRD patterns of the microwave irradiation assisted and non-microwave irradiation assisted nanopowders showed the coexistence of hydroxyapatite (HA) and tricalcium phosphate (TCP) phases in the system.     

Growth and characterization of large, high quality cubic diamond crystals

High quality cubic diamond crystals were grown using the temperature gradient method at high pressure and high temperature(HPHT),in a new FeNi alloy as solvent.The crystals were grown at relatively low temperatures suitable for the growth of {100} faces.An increase in the radial growth rate,and inhibition of the axial growth caused the growth of large,high quality cubic diamond single crystals at high growth rates.For example,over 33 h,the radial growth rate was 0.22 mm/h,while the axial growth rate was only 0.08 mm/h;the growth rate by weight was also increased to 7.3 mg/h.The yellow color of our crystal samples was more uniform than samples from Sumitomo Corporation of Japan and Element Six Corp.The Raman FWHW of the 1332 cm 1 peak in our diamond sample was smaller than the Element Six Corp.sample,but larger than that of the Sumitomo Corp.sample.The nitrogen content of our diamond samples was 240 ppm,which was much higher than the Sumitomo and Element Six samples because of the higher growth rate of our diamond samples.     

Nitridation of chromium powder in ammonia atmosphere

CrN powder was synthesized by nitriding Cr metal in ammonia gas flow, and its chemical reaction mechanism and nitridation process were studied. Through thermodynamic calculations, the Cr-N-O predominance diagrams were constructed for different temperatures. Chromium nitride formed at 7002-1200℃ under relatively higher nitrogen and lower oxygen partial pressures. Phases in the products were then investigated using X-ray diffraction (XRD), and the Cr₂N content varied with reaction temperature and holding time. The results indicate that the Cr metal powder nitridation process can be explained by a diffusion model. Further, Cr₂N formed as an intermediate product because of an incomplete reaction, which was observed by high-resolution transmission electron microscopy (HRTEM). After nitriding at 1000℃ for 20 h, CrN powder with an average grain size of 63 nm was obtained, and the obtained sample was analyzed by using a scanning electron microscope (SEM).     

Microwave sintering effects on the microstructure and mechanical properties of Ti-51at%Ni shape memory alloys

Ti-51at%Ni shape memory alloys (SMAs) were successfully produced via a powder metallurgy and microwave sintering technique. The influence of sintering parameters on porosity reduction, microstructure, phase transformation temperatures, and mechanical properties were investigated by optical microscopy, field-emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD), differential scanning calorimetry (DSC), compression tests, and microhardness tests. Varying the microwave temperature and holding time was found to strongly affect the density of porosity, presence of precipitates, transformation temperatures, and mechanical properties. The lowest density and smallest pore size were observed in the Ti-51at%Ni samples sintered at 900℃ for 5 min or at 900℃ for 30 min. The predominant martensite phases of β2 and β19' were observed in the microstructure of Ti-51at%Ni, and their existence varied in accordance with the sintering temperature and the holding time. In the DSC thermograms, multi-transformation peaks were observed during heating, whereas a single peak was observed during cooling; these peaks correspond to the presence of the β2, R, and β19' phases. The maximum strength and strain among the Ti-51at%Ni SMAs were 1376 MPa and 29%, respectively, for the sample sintered at 900℃ for 30 min because of this sample's minimal porosity.     

Size-manipulat ion, compacti on and electrical properties of barium manganite nanorods synthesized via the CHM method

A composite-hydroxide mediated method was employed to synthesize barium manganite nanorods.Diameter,surface smoothness and uniformity of these nanorods were optimized by varying reaction temperature and reaction time.The rods with an average diameter of 200 nm and length of1–1.5 μm were obtained at optimum conditions of 200 1C/48 h.The dielectric study of these rods reveals that they have higher value of dielectric constant at lower frequencies which was attributed to the interfacial and rotational type polarizations.Similarly,the increase in dielectric constant with temperature was attributed to the thermal activation of such polarizations.Furthermore,the analysis of ln(J) vs.E1/2characteristics in the temperature range of 300–400 K shows that possible operative conduction mechanism was of Poole–Frenkel type.The value of βexp was found to be 4.85 times greater than the expected theoretical value of feld lowering coeffcient with an internal feld enhancement factor ofα2 23.5.This high value of βexp may be due to some localized electric felds existing inside the sample.     

Effect of Sintering on Grain Boundary Microstructure and Electrical Properties of CaCu_3Ti_4O_(12) Ceramics

CaCu3Ti4O12 ceramic with a giant dielectric constant was synthesized by sol-gel method and sintered in three different sintering conditions: 1 035 ℃ for 48 h, 1 080 ℃ for 3 h and 48 h. The phase of the ceramics, the element distribution, the valance state of Ti ions at grain boundaries, and the electrical properties were characterized via X-ray diffraction(XRD), energy dispersive X-ray analysis(EDAX), X-ray photoelectron spectroscopy(XPS), electrical conduction and dielectric measurement. The results demonstrate that the grain-boundary microstructure and the electrical properties are influenced by sintering conditions: 1 By raising sintering temperature, the Cu-rich and Ti-poor grain boundary was formed and grain resistivity was decreased. 2 By prolonging sintering time, the content of Ti3+ near the grain boundary increased, leading to the decrease of the grain-boundary resistivity and the increase of the activation energy at grain boundary. The ceramic, sintering at 1 080 ℃ for 48 h, exhibited a small grain resistivity(60.5 *cm), a large grain-boundary activation energy(0.42 e V), and a significantly enhanced dielectric constant(close to 1×105 at a low frequency of 1×103 Hz). The results of electrical properties accord with the internal boundary layer capacitor model for explaining the giant dielectric constant observed in Ca Cu3Ti4O12 ceramics.     

Thermal degradation of BaAl2Si2O8：Eu2＋ phosphor excited by near ultraviolet light

Eu2+ doped BaAl2Si2O8 phosphor was synthesized by one-step calcination of precursors that were prepared by chemical co-precipitation.The thermal degradation properties of BaAl2Si2O8:Eu2+ were investigated by photoluminescence,lifetime and chromaticity coordinate measurements.BaAl2Si2O8:Eu2+ is efficiently excited by incident light of 250-400 nm,which matches the emission of near ultraviolet LED chips well.BaAl2Si2O8:Eu2+ exhibits broad blue emission at 470 nm because of the 4f65d1-4f7(8S7/2) transition of Eu2+ ions,and the emission band shows an unusual blue shift with bandwidth broadening and emission intensity decreasing as the annealing temperature is increased.The luminescence decay and CIE chromaticity coordinates of BaAl2Si2O8:Eu2+ were determined to investigate its application in white LEDs.     

Microstructure and properties of high emissivity coatings

A new coating on lining in industrial furnace for energy saving has been developed. Properties and microstructure of the coatings were revealed by emissivity instrument,X-ray diffraction (XRD),transmission electron microscope (TEM) and scanning electron microscope (SEM),respectively. The result indicates that the emissivity of coatings is higher than 0.90 and the thickness of coatings is about 200 μm. ZrO₂,Cr₂O₃ and SiC in the coating benefit practical applications of coatings at high temperature with durable high emissivity and the continuous structure between the coatings and the substrate makes the coatings high cohesion and excellent adhesion for both specimens with and without sintering at high temperature. Result from laboratory experiment shows that the heating speed of specimen with coating is higher than that of controlled specimen and the temperature increases 30℃ during the heating. The average temperature drop of specimen with coatings has a 13.5% improvement in the cooling speed. The application of coatings on the checker brick in a blast furnace of 1750m3 indicates that the coating causes the blast temperature to an average increase of 28℃,reduces the fluctuation of blast temperature before the blowing-in and leads to a fuel saving of 10% approximately.     

Linking leach chemistry and microbiology of low-grade copper ore bioleaching at different temperatures

The effects of temperature on chalcocite/pyrite oxidation and the microbial population in the bioleaching columns of a low-grade chalcocite ore were investigated in this study. Raffinate from the industrial bioleaching heap was used as an irrigation solution for columns operated at 20, 30, 45, and 60℃. The dissolution of copper and iron were investigated during the bioleaching processes, and the microbial community was revealed by using a high-throughput sequencing method. The genera of Ferroplasma, Acidithiobacillus, Leptospirillum, Acidiplasma, and Sulfobacillus dominated the microbial community, and the column at a higher temperature favored the growth of moderate thermophiles. Even though microbial abundance and activity were highest at 30℃, the column at a higher temperature achieved a much higher Cu leaching efficiency and recovery, which suggested that the promotion of chemical oxidation by elevated temperature dominated the dissolution of Cu. The highest pyrite oxidation percentage was detected at 45℃. Higher temperature resulted in precipitation of jarosite in columns, especially at 60℃. The results gave implications to the optimization of heap bioleaching of secondary copper sulfide in both enhanced chalcocite leaching and acid/iron balance, from the perspective of leaching temperature and affected microbial community and activity.     

Hydrogen storage of multiwalled carbon nanotubes coated with Pd-Ni nanoparticles under moderate conditions

A type of novel material with a high hy-drogen storage capacity was prepared by supporting PdNi18 alloy nanoparticles,which were synthesized by using a new colloid method,on the surface of pretreated multiwalled carbon nanotubes (MWCNTs). The average PdNi18 alloy particle sizes calculated from XRD patterns were ca. 3 nm,and the high dis-persion of these particles on MWCNTs was con-firmed by TEM image. Hydrogen storage perform-ance of the composite was investigated under mod-erate pressure (0.1―1.5 MPa) at room temperature,and a maximum storage capacity of ca. 2.3 wt% was achieved under 1.5 MPa at room temperature,which was much higher than that reported previously under the same conditions.     

Synthesis and characterization of monoclinic TiO<Subscript>2</Subscript> nanosheets

A novel two-step method for the synthesis of monoclinic titanium oxide （i.e. TiO2（B）） nanosheets is presented in this report. The method is featured by two steps： 1） synthesis of hydrogen titanate nanosheets, followed by 2） calcination of the titanate nanosheets at elevated temperatures. The hydrogen titanate nanosheets were prepared first by autoclaving anatase TiO2 powders, obtained by air cal- cining an ethanol-gel of Ti（OH）4 at 500℃, in aqueous NaOH （10 mol/L） at 150-200℃, and then by washing with hydro- chloric acid under supersonic irradiation. While sizes of the nanosheets were found to increase with increasing the temperature of the hydrothermal treatment, the calcination at 400-500℃ of the hydrogen titanate nanosheets that were synthesized at higher autoclaving temperatures （180-200℃） produced monoclinic TiO2 nanosheets with a uniform morphology. By contrast, the same calcination of the titanate nanosheets synthesized at the autoclaving temperature 180℃ led to anatase TiO2 nanoparticles.     

Effect of heating rate on the densification of NdFeB alloys sintered by an electric field

This study introduces a novel method of electric field sintering for preparing NdFeB magnets. NdFeB alloy compacts were all sintered by electric fields for 8 min at 1000℃ with different preset heating rates. The characteristics of electric field sintering and the effects of heating rate on the sintering densification of NdFeB alloys were also studied. It is found that electric field sintering is a new non-pressure rapid sintering method for preparing NdFeB magnets with fine grains at a relatively lower sintering temperature and in a shorter sintering time. Using this method, the sintering temperature and process of the compacts can be controlled accurately. When the preset heating rate increasing from 5 to 2000℃/s the densification of NdFeB sintered compacts gradually improves. As the preset heating rate is 2000℃/s, Nd-rich phases are small, dispersed and uniformly distributed in the sintered compact, and the magnet has a better microstructure than that made by conventional vacuum sintering. Also, the maximum energy product of the sintered magnet reaches 95% of conventionally vacuum sintered magnets.