Influence of B source materials on the synthesis of TiB2-Al2O3 nanocomposite powders by mechanical alloying

An Al2O3-TiB2 nanocomposite was successfully synthesized by ball milling of Al, TiO2 and two B source materials of B2O3 （system （1）） and H3BO3 （system （2））. Phase identification of the milled samples was examined by Xray diffraction. The morphology and microstructure of the milled powders were monitored by scanning electron microscopy and transmission electron microscopy. It was found that the formation of this composite was completed after 15 and 30 h of milling time in systems （1） and （2）, respectively. More milling energy was required for the formation of this composite in system （2） due to the lubricant properties of HaBO3 and also its decomposition to HBO2 and B2O3 during milling. On the basis of X-ray diffraction patterns and thermodynamic calculations, this composite was formed by highly exothermic mechanically induced self-sustaining reactions （MSR） in both systems. The MSR mode took place around 9 h and 25 h of milling in systems （1） and （2）, respectively. At the end of milling （15 h for system （1） and 30 h for system （2）） the grain size of about 35-50 nm was obtained in both systems.     

Selective catalytic oxidation of ammonia to nitrogen over orderly mesoporous CuFe2O4 with high specific surface area

Orderly mesoporous CuFe2O4 spinel-type mixed oxide with high specific surface area was prepared successfully by a hard-template method in which KIT-6 mesoporous silica was selected as the hard template. The KIT-6 hard template and CuFe2O4 samples were charac- terized by X-ray diffraction, X-ray photoelectron spec- troscopy, X-ray fluorescence, transmission electron microscopy, scanning electron microscopy, nitrogen physisorption, and hydrogen-temperature programmed reduction. The KIT-6 hard template had perfect crystalli- zation and ordered mesoporous structure with a probable pore distribution of about 9.1 nm, large enough to be filled by the spinel precursor. The mesoporous CuFe2O4 spinel oxide synthesized inside the KIT-6 mesopores had a rela- tively small pore size （4.3 nm）, orderly arrangement, and high specific area （194 m2/g）. The catalytic activity of the mesoporous CuFe2O4 was tested for the selective oxidation of ammonia to nitrogen. The conversion of ammonia reached nearly 100 % at 300 ℃with a nitrogen selectivity as high as 96 %. The nitrogen selectivity remained high with increasing temperature and even maintained a value of 80 % at 600 ℃.     

Surface modification of Ti-45Al-8.5 Nb alloys by microarc oxidation to improve high-temperature oxidation resistance

Microarc oxidation(MAO)electrolysis plasma deposition was used to prepare Al_2O_3coatings on Ti-45Al-8.5 Nb alloys to improve high temperature oxidation resistance.The surface and cross-section morphologies before and after high-temperature oxidation,the chemical composition,and the phase identification of the coatings were investigated by scanning electron microscopy(SEM),electron probe microanalyses(EPMA),and X-ray diffraction(XRD).The results show that Al_2O_3coatings with a thickness of approximately 8μm can be obtained on the Ti-45Al-8.5 Nb alloys by MAO for 600 s.The samples with the Al_2O_3coatings exhibited better high-temperature oxidation resistance.A minimal weight gain of only 0.396 g/m~2after 100 h oxidation at 900°C was observed for the coatings formed with a deposition voltage of 400 V and using a duty cycle of 3%.The deposition mechanism of the Al_2O_3coatings and the effect of the MAO parameters are also described.     

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.     

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.     

Effect of the synthesis route on the structural and dielectric properties of SrBi<Subscript>1.8</Subscript>Y<Subscript>0.2</Subscript>Nb<Subscript>2</Subscript>O<Subscript>9</Subscript> ceramics

This work is devoted to the synthesis and characterization of yttrium-doped SrBi₂Nb₂O₉ ceramics prepared by three methods: solid state reaction, co-precipitation, and hydrothermal. Multiple characterizations, specifically scanning electron microscopy (SEM), X-ray powder diffraction (XRD), and Fourier transform infrared spectroscopy (FTIR), were used to validate the structural feature. The crystallite size was estimated by Scherrer’s formula and the Williamson–Hall plot. The effect of the process on the band intensities of the FTIR spectra was investigated. The crystallite size and microstructure of ceramics prepared from different synthesis processes were strongly influenced by the sinterability. SEM images revealed nanograin ceramics for materials prepared by co-precipitation and hydrothermal methods and micrograin ceramics prepared by the solid state method. The synthesized compounds underwent phase transitions at 480–465°C. The dielectric and electrical properties of these Y-doped SrBi₂Nb₂O₉ ceramics appear to be dependent on the grain size.     

Solid electrolyte composite Li_4P_2O_7-Li_3PO_4 for lithium ion battery

The researches on solid electrolyte have been significantly increasing due to the safety problem in lithium ion battery.The lithium phosphates are chosen due to environmentally friendly.In the present study Li_4 P_2 O_7 was synthesized by solid state reaction using NH_4 H_2 PO_4 and Li_2 CO_3 with the ratio 1:2 at various temperatures of600 ℃,800 ℃ and 900℃.The products were characterized by x-ray diffraction,scanning electron microscopy and impedance spectroscopy.The x-ray diffraction showed that all samples consisted of two phases.It was found that the products consisted of 52.44% Li_4 P_2 O_7 and 47.56% LiPO_3;93.56% Li_4 P_2 O_7 and 6.44% Li_3 PO_4;and46.27% Li_4 P_2 O_7 and 53.67% Li_3 PO_4 under the synthesizing temperature of 600 ℃,800℃ and 900 ℃,respectively.The highest ionic conductivity of 3.85 ×10~(-5) S/m was achieved for composite Li_4 P_2 O_7-Li_3 PO_4 with the highest content of 93.56% Li_4 P_2 O_7.This conductivity is higher compared with single phase of LiPO_3,Li_3 PO_4 and Li_4 P_2 O_7.The increase in ionic conductivity may be due to the mixed anion effects related to the phosphate networks,and it also corresponds to the existence of anorthic phase Li_4 P_2 O_7 with the space group P-1(2).The crystal lattice analysis showed that the reactant Li_4 P_2 O_7 consisted of diphosphate groups P_2 O_7.The lithium tetrahedral LiO_4 were linked to P_2 O_7 groups formed a continuous framework containing large voids,available for Li~+ ion transport,and thus it exhibited high conductivity.A composite Li_4 P_2 O_7-Li_3 PO_4 is a promising solid electrolyte for solid state battery.     

Formation mechanism of an aluminium-based chemical conversion coating on AZ91D magnesium alloy

An environmentally clean aluminium-based conversion coating on AZ91D magnesium alloy was studied in aluminium nitrate solutions. The morphology, composition, structure, and formation mechanism of the coating were investigated in detail using scanning electron microscopy/energy dispersion spectrometry, X-ray diffraction, transmission electron microscopy, and electrochemical corrosion tests. The results show that the conversion coating is composed of magnesium, aluminium, and oxygen, and shows an amorphous structure. In the initial stage of coating formation, the grain-like nucleus is composed of Al₁₀O₁₅·xH₂O, (Al₂O₃)_5.333, Al₂O₃, AlO(OH), MgAl₂O₄, (Mg_0.88Al_0.12)(Al_0.94Mg_0.06)₂O₄, and (Mg_0.68Al_0.32)(Al_0.84Mg_0.16)₂O₄. The conversion coating formed in the 0.01 mol/L aluminium nitrate solution for 15 min can improve the corrosion resistance of the magnesium alloy greatly. The discussion reveals that the possible formation mechanism for the aluminium-based conversion coating is the reduction reaction on micro-cathodic sites due to the electrochemically heterogeneous magnesium alloy substrate.     

Template-free synthesis of morphology- and size-controlled nano indium hydroxide

Morphology- and size-controlled In(OH)₃ nanocrystals were synthesized via a novel, low-cost and low-temperature (70℃) route in the absence of any template and surfactant. The as-prepared products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and high-resolution transmission electron microscopy (HRTEM) with selected area electron diffraction (SAED). The morphology and size of In(OH)₃ nanostructures can be controlled by adjusting the reaction conditions such as the reaction time, the concentration of the alkali, and the alkaline source. A possible mechanism for the evolution of the morphology- and size-controlled In(OH)₃ was proposed. In addition, the optical properties of the In(OH)₃ prepared by this method were studied by diffuse reflection spectra (DRS) and photoluminescence (PL) spectroscopy, and the results exhibit an obvious change of adsorption edges. The thermal behaviors of the as-prepared products were also explored by thermo-gravimetric (TG) and differential scanning calorimetry (DSC) measurements. According to the results of TG-DSC, the pure phase and uniformity of the In₂O₃ nanocube and nanorod can be obtained by annealing In(OH)₃ precursors directly at 300℃.     

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…     

Effects of the hierarchical pyrolysis polyaniline on reversible hydrogen storage of LiBH4

In this work,LiBH_4–20 wt%PP composite was prepared by ball-milling with as-synthesized hierarchical pyrolysis polyaniline(PP)and LiBH_4,and the hydrogen sorption performance as well as catalytic mechanism of the composite was studied.It is found that the onset desorption temperature of the composite decreases to 75°C,almost 235°C lower than that of the milled LiBH_4.Moreover,the composite could release 4.1 wt%H_2and rehydrogenate a total of 4.4 wt%H_2when the temperature raiseds up to 400°C,showing an outstanding reversibility,which even 3.9 wt%H_2can be kept after five cycles.Through scanning electron microscopy(SEM)observation and X-ray diffraction(XRD)analysis,we found that the PP surface forms some nanoholes after hydrogenation-dehydrogenation cycles,which leads to the confinement of some LiBH_4in the PP nanoporous structure,therefore,the hydrogen sorption kinetics and reversibility are significantly enhanced.In addition,we also found the oxygenic groups of the PP can react with LiBH_4forming LiBO_2and Li_3BO_3,where the containing Li–B–O bonds loaded in the porous structure of the PP catalyze the hydrogenation reaction of LiBH_4.     

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.     

Preparation and magnetic properties of CoFe2O4/TiO2 composite films

Using （Ti（OC4H9）4） and metal chlorates as starting materials, CoFe2O4/TiO2 composite films were prepared by sol-gel method. The effects of heat treatment temperature and pH of the precursor on microstructure and magnetic properties were studied. The phase structure of the samples was examined by X-ray diffraction. The microstructure was examined by scanning electron microscope, atomic force microscope and polarized microscope. The magnetic property was measured by vibrating sample magnetometer. The results show that the crystals of different phases grow up independently. CoFe2O4 is uniformly embedded into the TiO2 matrix in the prepared composite films, and the growth of composite films is dependent on the heat treatment temperatures and PH of the precursor. The average size of CoFe2O4 crystal is 19 nm in Nanocomposite film prepared when the heat treatment temperature is 800℃ and the pH of the precursor is between 2 and 3. The magnetism of the composite films is enhanced as the heat treatment temperature increases.     

Effect of B2O3 on the aqueous tape casting and microwave properties of Li2O–Nb2O5–TiO2 ceramics

The effect of B2O3 addition on the aqueous tape casting, sintering, microstructure and microwave dielectric properties of Li2O-Nb2O5-TiO2 ceramics has been investigated. The tape casting slurries exhibit a typical shear-thinning behavior without thixotropy, but the addition of B2O3 increases the viscosity of the slurries significantly. It was found that doping of B2O3 can decrease the tensile strength, strain to failure and density of the green tapes. The sintering temperature could be lowed down to 900℃ with the addition of 2 wt% B2O3 due to the liquid phase effect. No secondary phase is observed. The addition of B2O3 does not induce much degradation on the microwave dielectric properties. Optimum microwave dielectric properties of εr 67, Q×f 6560 GHz are obtained for Li2O-Nb2O5-TiO2 ceramics containing 2 wt% B2O3 sintered at 900 1C. It represents that the ceramics could be promising for multilayer low-temperature co-fired ceramics (LTCC) application.     

Photocatalytic property of TiO2 sensitized by different crystal phase CdS

TiO2 samples sensitized by different crystal phase CdS(CT) are synthesized by hydrothermal process at different reaction temperature. The samples are characterized by X-ray diffraction(XRD), transmission electron microscopy(TEM), and UV-Vis diffuse reflectance(UV-Vis). The XRD result reveals that the crystal phase of CdS is transformed from cubic phase to hexagonal phase with the increase of hydrothermal reaction temperature(120-160 ℃). The absorption edge of CT is extended from 498 nm to 546 nm. The photocatalytic degradation of rhodamin B(RhB) in aqueous solution is used to evaluate the photocatalytic activity of CT. With the increase of the preparation temperature, the photocatalytic activity of CT becomes stronger. The degradation rate of RhB by CdS/TiO2 at 160 ℃(CT-160 ℃)reaches 78%.     

Simple point contact WO3 sensor for NO2 sensing and relevant impedance analysis

A simple and new point contact tungsten trioxide (WO₃) sensor, which can be prepared by the oxidation of tungsten filaments via in-situ induction heating, likely detects low concentration (ppm level) environmental pollutants such as NO₂. X-ray diffraction (XRD) and field emission scanning electron microscopy (FE-SEM) were applied to characterize the phase and the microstructure of the samples, respectively. It was found that the synthesized WO₃ films exhibited a monoclinic phase and were composed of hierarchical microcrystals and nanocrystals. The point contact WO₃ sensor (W-WO₃-W) showed rectifying characteristics and an ideal sensing performance of about 110°C. A single semicircle in Nyquist plots was recorded by electrochemical impedance spectroscopy (EIS) at a relatively low temperature of 150°C but faded away above 200°C, which revealed that the sensing process was governed by a determining factor, i.e., grain boundaries at the contact site.     

Structure evolution of Y2O3 nanoparticle/Fe composite during mechanical milling and annealing

Fe-25 wt% Y2O3composite powders have been fabricated by mechanical milling(MM) Fe powders of 100 μm in diameter and Y2O3nanoparticles in an argon atmosphere for the milling periods of4,8,12,24,36,and 48 h,respectively.The features of these powders were characterized by using X-ray diffraction(XRD),scanning electron microscopy(SEM),electron probe micro analyzer(EPMA) and transmission electron microscopy(TEM).The experimental results showed that the mean particle size and crystalline size of MM powders decreased with the milling time increasing.All the elements distributed homogenously inside the powders after 48 h of MM.The lattice constant of the matrix α-Fe kept constant with the milling time,and no solid solution took place during MM process.After 8 h of MM,the α-Fe in each powder became nanocrystalline.After 48 h of MM,Y2O3changes from nanostructure into amorphous structure,and the crystalline size of α-Fe further decreased to 10 nm.The Y2O3in the powders mechanically milled for 48 h kept the amorphous structure after being annealed at 400 1C,and starts to crystallize when the powders are annealed at 600 1C.The amorphous Y2O3contains a small amount of Fe,and crystalline FeYO3appears at 800 1C.     

Preparation of high emissivity NiCr<Subscript>2</Subscript>O<Subscript>4</Subscript> powders with a spinel structure by spray drying

Spray-drying was used to produce the high emissivity NiCr₂O₄ powders with a spinel structure. Preliminary investigations focused on fabricating the high emissivity powders for infrared radiation coatings and finding the relationship between microstructure and emissivity. The NiCr₂O₄ powders were characterized for composition, microstructure, and infrared emissivity by X-ray diffraction (XRD), scanning electron microscopy (SEM), infrared radiant instrument, and Fourier transform infrared spectra (FT-IR). Thermogravimetry and differential thermal analysis show that the appropriate baking temperature for NiCr₂O₄ powder preparation is about 1200°C. The emissivity measurement and FT-IR spectra show that, because of the special spinel structure, the NiCr₂O₄ powders have a high emissivity about 0.91. Spray-drying is a suitable method to produce the high emissivity ceramic powders.     

Fabrication and Photocatalytic Characteristics of TiO2 Films on Silicon Substrates

Silicon ( 111 ) and Silicon (100) have been employed for fabrication of TiO2 films by metal organic chemical vapor deposition (MOCVD). Titanium (Ⅳ) isopropoxide (Ti[O (C3H7)4 ])was used as a precursor. The as-deposited TiO2 films have been characterized with Field emission scanning electron microscopy (FE-SEM), X ray diffraction (XRD) and atomic force microscopy (AFM). The photocatalytic properties were investigated by decomposition of aqueous orange Ⅱ. The crystalline and structural properties of TiO2 film had crucial influences on the photodegradation efficiency. For MOCVD in-situ deposited films on Si substrates, thephotoactivities varied following a shape of “M”: At lower (350 ℃ ) middle (500 ℃) and higher (800 ℃) temperature of deposition, relative lower photodegradation activities have been observed. At 400 ℃ and 700 ℃ of deposition, relative higher efficiencies of degradation have been obtained, because one predominant crystallite orientation could be obtained as deposition at those two temperatures, especially a single anatase crystalline TiO2 film could be obtained at 700 ℃ growth.     

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).