Preparation and Characterization of Gd3Sc2Ga3O12 Polycrystalline Material by Co-Precipitation Method

Gd3Sc2Ga3O12 polycrystalline material for single crystal growth was prepared with Ga, Gd2O3 and Sc2O3 as starting materials and aqueous ammonia as the precipitator by co-precipitation method. The precursors sintered at various temperatures were characterized by infrared spectra （IR）, X-ray diffractometry （XRD） and transmitted electron microscopy （TEM）. The results showed that pure GSGG phase could be obtained at 900 ℃. The sintered powders were well-dispersed and less-aggregated in the sintered temperature range of 900 - 1000 ℃. XRD and TEM show that the polycrystalline particle sizes of the polycrystalline powders were about 20 - 50 nm. Compared with the method that Ga2O3, Gd2O3 and Sc2O3 were mixed directly and sintered to get polycrystalline materials, the synthesized temperature was lower and sintered time was shorter. Thus co-precipitation was a good method to synthesize GSGG polycrystalline material.     

Preparation of Sr_2Fe_(1-x)Sc_xMoO_(6-δ) nanopowders and its electrical conductivity

Double-perovskite Sr2Fe1-xScxMoO6-δ (x=0, 0.05, 0.1, 0.2, 0.3, 0.4) powders applied to the cathode of solid oxide electrolysis cells were synthesized by the sol-gel citrate combustion method. Initial powders were calcined at different temperatures under different atmosphere (air, H2(4 vol.%)/Ar), and the effects of the preparation process on the structure and the morphology of the powders were investigated by thermal analysis (TG/DSC), X-ray diffraction (XRD), scanning electron microscopy (SEM) and surface area analysis. The electric conductiv-ity of the materials was measured by electrochemical work station using wafers prepared by dry pressing. It was found that the formation of perovskite structure was related to the content of Sc and combustion improver (NH4NO3), pH value, calcining temperature and atmosphere. A single perovskite phase of Sr2Fe1-xScxMoO6-δ could be formed after 3 h calcining in reducing atmosphere of H2 (4 vol.%)/Ar at 1100 oC. The electrical property indicated that, this material had a potential to be used in medium/high temperature solid oxide fuel cells or electrolysis cells.     

Preparation of neodymium-doped yttrium aluminum garnet powders and fibers

Using nitrate precursors, a novel spray-drying assisted citrate gel process for the preparation of neodymium-doped yttrium alumi- num garnet （YAG） phase was developed. Synthesis of single-phase polycrystalline YAG was achieved at temperatures as low as 800 ℃ using the spray-drying methodology whilst conventional approaches currently available require 1000 ℃. Initially, a solution was prepared by mixing aluminum and yttrium nitrates, citric acid, etilenglycol and neodymium oxide. This solution was dried by pulverization （spray dryer） to obtain aggregated precursor powders of the compound. These aggregates were calcined at 800, 850 and 900 ℃ to determine the phase evolution from amorphous to crystalline by X-ray diffraction （XRD）. The morphology of aggregates was characterized by scanning electron microscopy （SEM） and transmission electron microscopy （TEM）. Moreover, through XRD it was determined that the crystallization of YAG phase started at about 800 ℃ without any intermediate phases. The powders were composed of spherical aggregates with an average diameter of 1 um. From these powders, ceramic fibers with additions of 2at.% and 5at.% Nd, were extracted from the melt with diameters ranging from 30 um to 50 um.     

Study on Agglomeration and Densification Behaviors of Gadolinium-Doped Ceria Ceramics

By synthesizing reactive powders via a self-sustaining combustion synthesis, the glycine-nitrate process, the gadolinium-doped celia （GDC） with the chemical formula Ce0.8Gd0.2O1.9 was prepared. The resultant powders were dispersed with the terpineol as the dispersant through different methods such as ball milling and high-shear dispersing. Coagulation factor （CF） was used to mark the degree of agglomeration on the nano-scale GDC in this work. The effect of agglomeration on the densification behavior at different sintering temperatures was investigated. The studies indicated that agglomeration retarded the densification at the sintering stage. The powders with better dispersion exhibited a higher sintered density at the same temperature. After effective dispersion treatment, GDC could be fully densified at the sintering temperature of 1300 ℃. The densification temperature was significantly lower than those reported previously. The high sintering kinetics of the ceramics was obtained based on the agglomeration control.     

Combustion synthesis and enhanced 1.5 μm emission in Y_2O_3:Er~(3+) powders codoped with La~(3+) ions

Er~(3+) and La~(3+) codoped Y_2O_3 nanocrystalline powders were synthesized by gel combustion method and characterized with thermal analysis, X-ray diffraction(XRD), transmission electron microscopy(TEM), high-resolution TEM(HRTEM) techniques and fluorescence spectroscopy. After being calcined at 1200 oC, the(Y_(1–x) La_x)_2O_3:Er~(3+) powders were confirmed to be cubic Y_2O_3 phase with the crystalline grain size in the range of 20–40 nm. The Er~(3+) emission at 1.53 μm from the ~4I_(13/2)→~4I_(15/2) transition was observed, which was found to be enhanced by introducing La~(3+) ions. Such enhancement could be attributed to the adjustment of Er~(3+) ions' local environment by the codoping of La~(3+) ions, leading to the increased ground state absorption cross section of Er~(3+) ions.     

Influence of laser re-melting and vacuum heat treatment on plasma-sprayed FeCoCrNiAl alloy coatings

FeCoCrNiAl high entropy alloy coatings were prepared by supersonic air-plasma spraying.The coatings were post-treated by vacuum heat treatment at 600 and 900°C,and laser re-melting with 300 W,respectively,to study the influence of different treatments on the structure and properties of the coatings.The phase constitution,microstructure and microhardness of the coatings after treatments were investigated using X-ray diffraction,scanning electron microscopy and energy dispersive spectrometry.Results showed that the as-sprayed coatings consisted of pure metal and Fe-Cr.The AlNi_3 phase was obtained after the vacuum heat treatment process.A body-centered cubic structure with less AlNi_3 could be found in the coating after the laser re-melting process.The average hardness values of the as-sprayed coating and the coatings with two different temperature vacuum heat treatments and with laser re-melting were 177,227,266 and 682 HV,respectively.This suggests that the vacuum heat treatment promoted the alloying process of the coatings,and contributed to the enhancement of the coating wear resistance.The laser re-melted coating showed the best wear resistance.     

Synthesis and photoluminescence properties of ZnTiO3:Eu3+ red phosphors via sol-gel method

ZnTiO3:Eu3+ phosphors were synthesized with different concentrations of Eu3+ doping through sol-gel method. The samples were calcined at different temperatures for 2 h in air. The synthesized powders were characterized by X-ray diffraction(XRD), scanning electron microscopy-energy dispersive spectroscopy(SEM-EDS), transmission electron microscopy(TEM), Raman and photoluminescence spectroscopy. The XRD results showed that the Zn Ti O3:Eu3+ phosphors doped with different concentrations of Eu3+ ions calcined at 600 oC were of single phase, which indicated that the Eu3+ ions had been successfully incorporated into the Zn Ti O3 host lattice and did not destroy the lattice structure of Zn Ti O3 host. The Raman spectrum, SEM and TEM also proved that the doping of Eu3+ did not change the lattice structure of hexagonal Zn Ti O3 host. The photoluminescence(PL) of Eu3+ ions with the main emission peak at 614 nm was observed to increase with Eu3+ concentrations from 0.5 mol.% to 2.0 mol.% and decreased when the concentration was increased to 2.5 mol.%. The decrease in the PL intensity at higher Eu3+ concentrations could be associated with concentration quenching effect. The CIE1931 chromaticity diagram(x, y) of Zn Ti O3:2.0 wt.%Eu3+ phosphors were located in the red region(x=0.652, y=0.347). The luminescence properties suggested that Zn Ti O3:Eu3+ phosphors might be regarded as a potential red phosphor candidate for light emitting diodes(LEDs).     

Structure and permanent magnetic properties of SmFex （x=3-8） melt spun ribbons during heat treatment

Compounds with the composition SmFex（x=3–8） were prepared by melt spun method at a velocity of 40 m/s and subsequent annealing at temperature between 600–1000 ℃. The crystal structures of the as-quenched and as annealed powders were investigated by XRD methods with following Rietveld analysis. The glass forming ability could be enhanced by the increase of Sm content to x≤5.Metastable Sm5Fe17-type structure existed when 3≤x≤5 and temperature was lower than 800 ℃. SmFe2-type structure could be stable up to 1000 ℃ when x〉3 and temperature was under 800 ℃. The content of SmFe2-type decreased with the increase of x value and increased with temperature lower than 800 ℃, from which SmFe2-type started to bring the transition to SmFe3-type. As for Sm5Fe17-type compounds with x=3.4, the highest coercivity of 33.6 kOe could be obtained under a velocity of 30 m/s and heat treated under 700 ℃×1h.     

Combustion synthesis and stability of nanocrystalline La2O3 via ethanolamine-nitrate process

Pure nanocrystalline La2O3 powders were successfully prepared by the combustion method.The effect of ethanolamine-to-nitrate ratio on phase composition and crystallite size of the combustion products was systematically investigated.Pure hexagonal La2O3 powders were almost formed in stoichiometric reaction(ψ=1.15),while metallic La phase was obtained in fuel-rich conditions(ψ≥3.0).The as-synthesized hexagonal La2O3 was found to be chemically unstable in ambient air since a complete transformation to hexagonal La(OH)3 was detected after 24 h exposure to air.The resulting hexagonal La(OH)3 showed an excellent ability to remove water pollutant and could nearly remove 100% of the Congo red at room temperature with a removal capacity of 143.5 mg Congo red/g.The phosphate adsorption data on hexagonal La(OH)3 agreed well with the Langmuir model with the estimated maximum adsorption capacity of 57.8 mg/g.     

Highly transparent ytterbium doped yttrium lanthanum oxide ceramics

To prepare ytterbium doped lanthania yttria nanopowder a method of laser evaporation of mixed oxides was used. After calcinations of the powder at 1200 °C a pure single-phase solid solution Yb3+:(LaxY1–x)2O3 was formed in the nanoparticles. Influence of lanthanum oxide as an isovalent additive on the yttria structure was investigated. The lanthanium ions were proved to be a good aid to sinter yttria ceramics doped with Yb3+ at moderate temperatures about 1650 °С. The ceramics with relative density higher than 99.99% and grain size about 40 μm were fabricated. Full transmittance of 1.8 mm thick Yb0.11La0.23Y1.66O3 ceramics reached 82.5% at 800 nm. This material could be a good gain medium for ytterbium high power pulse lasers.     

Solution-Phase Synthesis and Characterization of Perovskite LaCoO3 Nanocrystals via A Co-Precipitation Route

A facile co-precipitation route for the synthesis of well-dispersed LaCoO3 nanocrystals was developed. The asprepared products were characterized by X-ray diffraction （XRD）, transmission electron microscopy （TEM）, energy dispersive X-ray spectrometer （EDX）, and laser Raman spectroscopy （LRS）. The resuks showed that modulating the growth parameters, such as the addition of surfactants as well as the adding manner of the precipitator had a significant effect on the overall shape and size of the obtained nanocrystals. The nanorods with the diameter of 20 nm and spherical LaCoO3 nanocrystals with the size of about 25 nm could be obtained at a relatively low calcining temperature of 600℃. Furthermore, the Raman properties of LaCoO3 products obtained at different calcining temperatures were investigated.     

Preparation and Characterization of Y_3Sc_2Ga3O（12） Nano-Polycrystalline Powders by Co-Precipitation Method

In order to grow high-quality gallium garnet crystals,polycrystalline materials were used as starting materials.YSGG precursor was synthesized by co-precipitation method using aqueous ammonia as a precipitator,and the precursor was then sintered at different temperatures.The results showed that the feasible pH range was 8.3～9.84 in the process of co-precipitation reaction.The YSGG precursor and the powders sintered at different temperatures were characterized by IR,XRD and TEM methods.It was found that the precursor transformed to pure YSGG polycrystalline phase at 800 ℃.YSGG nano-polycrystalline powders sintered at 800～1000 ℃ were well dispersed and the sizes of the YSGG grains were about 40～100 nm.     

Preparation and characterization of Ce_1-xNi_xO₂ as oxygen carrier for selective oxidation methane to syngas in absence of gaseous oxygen

A citric acid complex method was employed to prepare Ce/Ni mixed oxides with various Ce/Ni ratios useful for selective oxidation methane to syngas in the absence of gaseous oxygen,and the catalytic activity measurement was investigated in a fixed bed reactor at 800 oC.The prepared oxygen carriers were characterized by various characterization techniques such as TG-DSC,XRD and TPR.The results of TG-DSC indicated that the Ce1-xNixO2 precursor generated a stable phase after the heat-treatment at temperatures above 800 oC.The XRD characterization suggested that some Ce-Ni solid solution was formed when Ni2+ ions was incorporated into the lattice of CeO2,and it led to the generation of O-vacancy which could improve the oxygen mobility in the lattice of oxygen carriers.It was found that Ce0.8Ni0.2O2 gave the highest activity in the selective oxidation methane to syngas reaction,and the average methane conversion,CO and H2 selectivity reached to 82.31%,82.41% and 87.64%,respectively.The reason could be not only attributed to the fitting amount of NiO dispersed on the CeO2 surface and bulk but also to actual lattice oxygen amount increased in oxygen carrier.     

Field emission from one-dimensional single-crystalline NdB6 nanowires

A facile catalysis-free method was utilized to synthesize functional neodymium hexaboride (NdB6 ) nanowires of single crystal using Nd powders and BCl 3 as starting materials. The XRD pattern confirmed that a single phase NdB 6 could be obtained. Raman-spectra elucidated the active vibrational modes of the hexaborides. The TEM images clearly showed that the hexaborides were submicron in size with a cubic morphology. The field emission of these one-dimensional NdB6 nanowires showed a low field emission turn-on (5.55 V/μm at a current density of 10 μA/cm2 ), and high current density with a field enhancement factor of 1037. The emission current density and the electric field followed the Fowler-Nordheim (F-N) relationship. The good performance for field emission was attributed to the single-crystalline structure and the nanowire geometry.     

Influence of concentration and sintering temperature on luminescence properties of Eu^3＋：SnO2 nanocrystallites

The nanopowders of SnO2 doped with different Eu3+ concentrations were synthesized using the modified Pechini method. The Eu3+ concentrations were high above solubility limit. The average size of crystallites was controlled by the sintering temperatures. The structure and the morphology of obtained powders were examined using the XRD (X-ray diffraction) and TEM (transmission electron microscopy) analyses. The Eu2Sn2O7 phase separation was observed at relatively high concentration of Eu3+ ions. The ZnS:Ag micropowders were mixed with the Eu3+:SnO2 powders and their normalized emission was used to measure a relative efficiency of Eu3+:SnO2. The photoluminescence spectra of mixed powders were measured in function of Eu3+ concentration and average size of nanocrystallites. The reference peak method was used for comparison of intensities of the samples and selection of optimal one. The influence of the average grain size and Eu3+ concen-tration on the phosphor’s efficiency was discussed. The presented results confirmed the rightness of synthesis of the Eu3+:SnO2 in form of nanocrystalites with relatively high Eu3+ concentration.     

Synthesis and characterization of calcium and manganese-doped rare earth oxide La_(1-x)Ca_xFe_(0.9)Mn_(0.1)O_(3-δ) for cathode material in IT-SOFC

In order to develop novel cathode materials with high performance for intermediate temperature SOFC(IT-SOFC),Ca and Mn doped rare earth oxides La1-xCaxFe0.9Mn0.1O3-δ(x=0.1,0.3 and 0.5,denoted as LCFM9191,LCFM7391 and LCFM5591) were synthesized by solid state reaction(SSR) method.The formation process,phase structure and microstructure of the synthesized samples were characterized using thermogravimetry/differential scanning calorimetry(TG/DSC),X-ray diffraction(XRD) and scanning electron microscopy(SEM).The thermal expansion coefficients(TEC) of the samples were analyzed at 100-900 oC by thermal dilatometry.The electrical conductivities of the samples were measured with direct current(DC) four-terminal method from 300 to 850 oC.The results indicated that the samples(x=0.1 and 0.3) exhibited a single phase with orthorhombic and cubic perovskite structure,respectively after being sintered at 1200 oC for 3 h.The electrical conductivity of the samples increased with temperature up to a maximum value,and then decreased.The small polaron hopping was regarded as the conducting mechanism for synthesized samples at T≤600 oC.The negative temperature dependence occurring at higher temperature was due to the creation of oxygen vacancies for charge balance.LCFM7391 had higher mixed conductivity(>100 S/cm) at intermediate temperature and could meet the demand of cathode material for IT-SOFC.In addition,the average TECs of LCFM9191 and LCFM7391 were 11.9×10-6 and 13.1×10-6 K-1,respectively,which had good thermal match to the common electrolytes.     

Highly nonlinear property and threshold voltage of Sc2O3 doped ZnO-Bi2O3-based varistor ceramics

A series of ZnO-Bi2O3-based varistor ceramics doped with 0-0.4 mol.% Sc2O3 were prepared by high-energy ball milling and sintered at temperatures between 1000 and 1150oC. X-ray diffractometry (XRD) and scanning electron microscopy (SEM) were applied to characterize the phases and microstructure of the varistor ceramics. A DC parameter instrument for varistor ceramics was applied to investigate the electronic properties and V-I characteristics. The results showed that there were no changes in crystal structure with Sc2O3-doped varistor ceramics and that the average size of ZnO grain increased first and then decreased. The best electronic characteristics of the varistor ceramics prepared by high-energy ball milling were found in 0.3 mol.% Sc2O3-doped ZnO-Bi2O3 -based ceramics sintered at 1000 oC, which exhibited a threshold voltage of 821 V/mm, nonlinear coefficient of 62.1 and leakage current of 0.16 μA.     

Hydrogen disproportionation phase diagram and magnetic properties for Nd_(15)Fe_(79)B_6 alloy

Transformation-temperature-hydrogen pressure phase diagram was constructed for a Nd_(15)Fe_(79)B_6 alloy in order to estimate appropriate conditions for hydrogenation, disproportionation, desorption and recombination reaction(the HDDR). Optimised recombination time(the highest coercivity) was found to be 10 min. for 5 g samples processed at 740 oC. Several HDDR processes were carried out at 30 kP a of hydrogen pressure at various temperatures. No correlation between magnetic propertiec and a direction of measurement was observed for the samples processed at 740 oC. Remanence anisotropy was induced along an alignment direction when the temperature of the HDDR process was increased up to 800 oC and 850 oC for 100 μm and 100–160 μm particles, respectively. Simultaneously, a small drop in coercivity was observed in the direction of alignment for 100 μm particles, but no for 100–160 μm particles. Furthermore, probably an ordered phase was found by TEM microstructure analysis in the bulk sample disproportionated at 850 oC under 150 kP a of hydrogen. Grains with antiphase domains were observed and corresponding electron diffraction patterns were resolved, likely indicating superlattice structures.     

Phase-, shape- and size-controlled synthesis of NaYF4：Yb3＋,Er3＋ nanoparticles using rare-earth acetate precursors

Hexagonal-phase NaYF4：Yb3＋,Er3＋ upconversion nanoparticles（UCNPs） with a uniform size distribution were synthesized using rare-earth acetates as precursors. The effects of reaction temperature and time on the phase transition process of the UCNPs were systematically studied. Based on the evolution of particle morphology and phase with temperature and time, it could be concluded that the transition from cubic phase to hexagonal phase for NaYF4：Yb3＋,Er3＋ UCNPs was consistent with a dissolution/recrystallization process. In addition, the shape and size of the UCNPs could be controlled by adjusting the solvent ratio and the precursor ratio, respectively.     

Stamping Formability of ZEIO Magnesium Alloy Sheets

ZE10 magnesium alloy sheets were prepared through ingot casting and the hot-rolling process. The mechanical properties, conical cup value （CCV）, bore expanding performance, and limit drawing ratio （LDR） were investigated to examine the stamping formability of ZE10 alloy sheets, at temperatures ranging from 20 to 300℃. The results showed that the tensile strength decreased, whereas, plasticity, drawing-bulging performance, bore expanding properties, and deep drawing performance increased markedly at elevated temperatures. The CCV specimens could be drawn into the conical die＇ s underside cylindrical hole from the conical cliff, without cracking, and could have the minimum CCV at 200 and 250 ℃ In the bore-expanding test, the bore （φ10 mm） could be expanded to the dimension of the punch （φ25 mm） and the maximum bore-expanding ratio could be achieved at above 150℃. The limiting drawing ratio （LDR） of 2.85 is acquired during the deep drawing test at 230 v with the punch temperature of 20 - 50℃, the punch velocity of 50 mm · min^-1, and the mixture of graphite and cylinder grease as lubricant.