Microwave sintering of Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-ZrO<Subscript>2</Subscript>-WC-Co cermets

Composite powders of nanocrystalline WC-10Co (15wt%),Y2O3 (8mol%) stabilized nanocrystalline ZrO2 (30wt%),industrial cobalt powder (4.5wt%) and submicron Al2O3 (55wt%) composite powders were fabricated by high-energy ball-milling process.The nanocomposite powders were consolidated by microwave sintering process at temperature ranged 1300℃-1550℃ for 15min,respectively.The optimum consolidation conditions,such as temperature,were researched during microwave sintering process.Vickers Hardness of the consolidated cermets was measured by using a Vickers indentation test,and density of specimens was also determined by Archimedes’ principle.Microwave sintering process could not only increase the density of Al2O3-ZrO2-WC-Co cermets and reduce the porosity,but also inhibit abnormal grain growth.     

Hydrothermal preparation and photocatalytic water splitting properties of ZrW<Subscript>2</Subscript>O<Subscript>8</Subscript>

ZrW₂O₈ was prepared by adjusting Zr:W mole ratio and HCl concentration in hydrothermal reaction processes. The obtained sample was crystallized in α-ZrW₂O₈ phase (cubic, P2₁3), with band gap energy of 4.0 eV. The properties of photocatalytic water splitting were examined under UV light irradiation. The average rate of H₂ evolution over 0.3wt% Pt/ZrW₂O₈ in the presence of CH₃OH as electron donor (ED) was 23.4 μmol/h, while the average rate of O₂ evolution over ZrW₂O₈ in the presence of AgNO₃ as electron scavenger (ES) was 9.8 μ mol/h. Moreover, H₂ was evolved over 0.3wt% Pt/ZrW₂O₈ from pure water splitting at a rate of 5.2 μ mol/h. The study indicated that the band structure of ZrW₂O₈ was suitable for reducing H⁺ to H₂ and oxidizing H₂O to O₂. The band structure and photocatalytic water splitting properties of ZrW₂O₈, different from either ZrO₂ (5.0 eV) or WO₃ (2.7 eV), were attributed to the hybridization of W5d and Zr4d in conduction band (CB) as well as the change in crystal structure.     

Co-precipitation/hydrothermal synthesis of BiFeO<Subscript>3</Subscript> powder

A coprecipitation/hydrothermal route was utilized to fabricate pure phase BiFeO3 powders using FeCl3·6H2O and Bi（NO3）3·5H2O as starting materials, ammonia as precipitant and NaOH as mineralizer. The synthesized powders were characterized by XRD, SEM and DSC-TG analysis. In the process, single-phase BiFeO3 powders could be obtained at a hydrothermal reaction temperature of 180 ℃, with NaOH of 0.15 mol/L, in contrast to 200 ℃ and 4 mol/L for conventional hydrothermal route. Meanwhile, the micro-morphology of synthesized BiFeO3 powders changed with different reaction temperatures and concentrations of NaOH. The N6el temperature, Curie temperature and decomposition temperature of the synthesized BiFeO3 powders were detected to be 301 ℃, 828 ℃ and 964 ℃, respectively. The hydrothermal reactions mechanism to fabricate BiFeO3 powders were discussed based on the in-situ transformation process.     

Stability of titanium-aluminium nitride (Ti<Subscript>2</Subscript>AlN) at high pressure and high temperatures

The stability of Ti2AlN at high pressure of 5 GPa and different temperatures of 700-1 600 ℃ was investigated using X-ray diffraction (XRD),scanning electron microscopy (SEM) equipped with an energy dispersive spectrometer (EDS).Ti2AlN was found to be stable at temperatures as high as 1 400 ℃under 5 GPa for 20 min,and was proved that it held better structure stability than Ti2AlC under 5 GPa through comparative experiments of Ti2AlN and Ti2AlC (representative compounds of M2AX phases (211 phase)).The reaction process at high pressure had some difference from that at ambient pressure/vacuum,and Ti2AlN directly decomposed to TiN and TiAl at 5 GPa and 1 500 ℃ for 20 min.Moreover,the mechanism of phase segregation was discussed.In addition,the behavior of Ti2AlN contacting with Zr at high pressure and high temperature (HPHT) was also studied.     

Preparation and microstructure of spinel zinc ferrite ZnFe<Subscript>2</Subscript>O<Subscript>4</Subscript> by Co-precipitation method

Spinel zinc ferrites ZnFe₂O₄, prepared by co-precipitation method using the zinc nitrate Zn(NO₃)₂·6H₂O and ferric nitrate Fe(NO₃)₃·2H₂O as the raw materials, were characterized by the thermo gravimetric analysis (TG) and differential scanning calorimeter (DSC), X-ray diffraction (XRD) and scanning electron microscope (SEM). The influence of synthesis conditions, such as Zn/Fe molar ratio, pH value, the sintering temperature and time, on the microstructures was detailedly investigated. The relationships between the microstructures and the synthesis conditions were discussed. The results show that the pure spinel zinc ferrites ZnFe₂O₄ are formed when the Zn/Fe molar ratio is 1.05:2 at pH=8.5 or Zn/Fe molar ratio is 1:2 at Ph=9-10, and the precursors are sintered at 1100 °C for 4 h. Especially no other phases are observed when the Zn/Fe molar ratio is 1:2 at pH=10 and the precursor is sintered above 700 for 4 °C h. The higher sintering temperature and longer sintering time contribute to grain growth.     

Low-temperature sintering and microwave dielectric properties of Ba<Subscript>2</Subscript>Ti<Subscript>3</Subscript>Nb<Subscript>4</Subscript>O<Subscript>18</Subscript> ceramics

The effects of CuO and H3BO3 additions on the low-temperature sintering,microstructure,and microwave dielectric properties of Ba2Ti3Nb4O18 ceramics were investigated.The addition of less amount of CuO (< 1 wt%) considerably facilitated the densification of Ba2Ti3Nb4O18 ceramics.Appropriate addition of H3BO3 (< 3.5 wt%) remarkably improved the microwave dielectric properties of ceramics.The addition of H3BO3 and CuO successfully reduced the sintering temperature of Ba2Ti3Nb4O18 ceramics from 1300 to 1050 ℃.B...     

Self-assembled SnO<Subscript>2</Subscript> colloidal particles and their gas sensing performance to H<Subscript>2</Subscript>, C<Subscript>2</Subscript>H<Subscript>5</Subscript>OH and LPG

Using organo-tin Sn(OC4H9)4 as precursor, sodium dodecyl sulfonate (SDS) and SDS-gelatin (SDS-G) complex as template, two tin dioxide colloidal particles were prepared by a self-assembly method. Both SnO2 products were respectively labelled SnO2-B particles with SDS and SnO2-C particles with SDS-G, which are applied in fabricating SnO2 gas sensors corresponding to SnO2-B’ and SnO2-C’ sensors. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and thermo-gravimetry and different thermal analysis (TG/DTA) were used for characterizations. The experimental results show that SnO2-B colloidal particles are composed of mesoporous piece-like particles, while SnO2-C particles mainly consist of spherical particles. Gas sensing measurements show that SnO2-B’ sensor performs the best sensing response to all target gases, including H2, C2H5OH and liquid petroleum gas (LPG). In particular, the sensing response of SnO2-B’ sensor is achieved at 32 in H2 atmosphere at the concentration of 1000×10-6 M. The gas sensing mechanism was purposely discussed from the electron transfer process and the microstructures of the as-prepared SnO2 products. It is found that serious agglomerations in SnO2-B’ particles facilitate the high gas sensing performance of SnO2-B’ sensor, while mesoporous structures in SnO2-C’ particles decrease the gas sensing response of SnO2-C’ sensor.     

Synthesis and photocatalytic property of the ZrO<Subscript>2</Subscript>/TiO<Subscript>2</Subscript> pillared laponite

The ZrO2/TiO2 pillared laponite (Ti-Zr-lap) photocatalysts were prepared with intercalation reaction by supercritical fluid drying (SCFD),and characterized by XRD,TEM,SEM and BET surface area analysis,and the photocatalytic properties of Ti-Zr-lap were investigated by degradation of azo dye acid red B (ARB).The results showed that the ZrO2/TiO2 pillared structures in laponite could be formed,with the mass fraction of (Zr4++Ti4+)/laponite (Xm) increasing,the basal spacing and the BET surface area of Ti-Zr-lap significantly increased.The Ti-Zr-lap used as photocatalyst had the advantages of stable and porous layered structure,large surface area with the anatase type TiO2.Compared with the Ti-Zr-lap dried by air drying,the Ti-Zr-lap dried by SCFD showed better photocatalytic property which was very close to that of P25 TiO2.Using the Ti-Zr-lap as photocatalyst with the optimum Xm of 0.16 and the calcination temperature of 500 ℃,under the conditions of the initial concentration of ARB 20 mg/L,photocatalyst concentration of 1.5 g/L and irradiation time 60 min,the decoloring rate of ARB could achieve 98.3%,indicating that the Ti-Zr-lap had excellent photocatalytic property.     

Controlled preparation of monodisperse CoFe<Subscript>2</Subscript>O<Subscript>4</Subscript> nanoparticles by a facile method

CoFe2O4 nanoparticles (NPs) were synthesized by coprecipitation method using FeCl3·6H2O and CoCl2·6H2O as precursors.The synthesized conditions were optimized,such as added means of precipitator,quantity of precipitator,the mol ratio of Fe 3+ to Co2+,reaction temperature and pH value.The synthesized material was characterized by XRD,TEM,FTIR,EDS,Raman and its magnetic properties were studied by VSM.The experimental results confirm that the sample is cubic spinel structure CoFe2O4 with a narrow size distribution and a good dispersion feature.CoFe2O4 NPs with well-controlled shape and size was obtained at 70℃.The magnetic properties indicate superparamagnetic behavior and good saturated magnetization.     

Manufacture Process of 8Y2O3 Stabilized ZrO2 from Nano Powders

The manufacture process of 8 mol% Y2O3 stabilized ZrO2 ( YSZ ) from nano powders, including the forming and sintering stages, was studied. During the forming process of YSZ powders, the relative density of YSZ increases lineally with the forming press, and the sintering linear shrinkage of YSZ to the forming press compiles to the parabola trend. When the forming press exceeding 500MPa, the samples with lower shrinkage and high density were obtained. The sintering temperature of YSZ decreases greatly because of the small size and high active surface of YSZ powders. As a result, the beginning sintering temperature of YSZ made in the experiment is as low as 825℃, and the end sintering temperature is 1300-1350℃ . The relative density of YSZ ceramic by solid sintering at 1300-1350℃ is more than 97% , with little and small pores in the uniform microstructure.     

Synthesis and characterization of biomimetic Fe<Subscript>3</Subscript>O<Subscript>4</Subscript>/coke magnetic nanoparticles composite material

A composite material (Fe₃O₄/Coke) using coke supported Fe₃O₄ magnetic nanoparticles was successfully prepared via an in-situ chemical oxidation precipitation method and characterized by SEM, XRD, Raman, and FTIR. The results showed that the Fe₃O₄ nanoparticles existed steadily on the surface of coke, with better dispersing and smaller particle size. The catalytic ability of Fe₃O₄/Coke were investigatied by degrading p-nitrophenol (P-NP). The results showed that the apparent rate constant for the P-NP at 1.0 g·L^?1 catalyst, 30 mmol·L^?1 H₂O₂, pH=3.0, 30 °C and the best ratio of Coke/Fe₃O₄ 0.6, was evaluated to be 0.027 min^–1, the removal rate of COD_Cr was 75.47%, and the dissolubility of Fe was 2.42 mg·L^–1. Compared with pure Fe₃O₄, the catalytic ability of Fe₃O₄/Coke in the presence of H₂O₂ was greatly enhanced. And Fe₃O₄/Coke was a green and environmental catalyst with high catalytic activity, showing a good chemical stability and reusability.     

Tensile properties of an aluminum matrix composite reinforced by SnO<Subscript>2</Subscript>-coated Al<Subscript>18</Subscript>B<Subscript>4</Subscript>O<Subscript>33</Subscript> whisker

Al18B4O33 whisker was coated by SnO2 particles using a chemical precipitation method, and an aluminum matrix composite reinforced by the coated whisker was fabricated by squeeze casting technique. It is found that the SnO2 coating can react with aluminum matrix during squeeze casting process, and Sn particles are induced near the interface between Al18B4O33 whisker and matrix. The tensile test at room temperature indicated that the tensile strength of Al18B4O33 whisker reinforced aluminum matrix composite can be enhanced by suitable content of SnO2 coating. The composites with various whisker coating contents exhibit maximum tensile plasticity at about 300 ℃, and the composite with a suitable whisker coating content could enhance its tensile plasticity evidently, which suggest that an Al18B4O33 whisker-Al composite with both high strength at room temperature and high formability at elevated temperature can be designed.     

Wear performance of Ni/ZrO<Subscript>2</Subscript> infiltrated composite layer

The Ni/ZrO2 was used as raw materials to fabricate the surface infiltrated composite layer with 1-4 mm thickness on cast steel substrate through vacuum infiltrated casting technology. The microstructure indicated that the infiltrated composite layer included surface composite layer and transition layer. Wear property was investigated under room temperature and 450 ℃. The results indicated that the abrasion volume of substrate was 8 times that of the infiltrated composite layer at room temperature. The friction coefficient of infiltrated composite layer decreased with the increasing load. The wear resistance of infiltrated composite layer with different ZrO2 contents had been improved obviously under high temperature. The friction coefficient of infiltrated composite layer was decreased comparing with that at room temperature. The oxidation, abrasive and fatigue abrasion was the main wear mechanism at room temperature. Oxidation abrasion, fatigue wear and adhesive wear dominated the wearing process under elevated temperature.     

Phase structure and electrical properties of La<Subscript>2</Subscript>O<Subscript>3</Subscript>-doped BiInO<Subscript>3</Subscript>-PbTiO<Subscript>3</Subscript> ceramics with high curie temperature

The phase structure and electrical properties of pure and La2O3-doped Bi-InO3-PbTiO3 （BI-PT） ceramics were studied respectively. In （1 -x）BI-xPT （x=0.72-0.80） ceramics, the stability of tetragonal phase increased with increasing x, and pure perovskite structure was obtained for x=-0.80 ceramics. The phase transition temperature range was between 575 ℃ and 600 ℃ for x=0.72-0.80 ceramics, higher than that of PT （-490 ℃）. The c/a ratio almost linearly decreased with increasing La2O3 content in x-0.80 ceramics. It is believed that Pb^2＋ vacancies were formed by La^3＋ substituting Pb^2＋ in La2O3-doped BI-PT ceramics. Tc shifted to lower temperature by 30 ℃/mol% La2O3. The maximum dielectric constant 8557 around 559 ℃ was exhibited in 0.5mol%-doped BI-0.80PT ceramics. La2O3-doped ceramics could be poled resulting from decreasing of c/a ratio and improving of dielectric loss and resistivity. The maximum piezoelectric coefficient d33 was 12 pC/N for 2mol%-doped BI-0.80PT ceramics.     

Effect of Mg/Al ratios on hydration mechanism of tabular alumina carbon composites reinforced by Al<Subscript>4</Subscript>C<Subscript>3</Subscript> in situ reaction

Hydration mechanism of tabular alumina carbon composites reinforced by Al₄C₃ in situ reaction with Mg and Al was researched in water steam using super automatic thermostatic water bath from 25 °C to 85 °C. It is shown that hydration mechanism of the composites is chemical reaction control at 44.3 °C-84 °C in H₂O(g). The hydration was controlled by diffusion from 24.7 °C to 33 °C. The ratio of added Mg/Al influences the HMOR of the composites.The mechanism of HMOR of the composites with different ratios of Mg/Al can be discovered by means of SEM analysis. The active Mg/Al powder and flake graphite inside give the composites outstanding hot strength resulting from the interlocking structure of Al₄C₃ crystals at high temperature. Besides, the matrix changes into the Al₄C₃ with high refractoriness. The method of preventing the hydration of tabular alumina carbon composites reinforced by Al₄C₃ in situ reaction was immersed in the wax at suitable temperature or storing them below 33 °C in a dry place or storing them with paraffin-coating.     

Sensing characterization of Sn/In/Ti nanocomplex oxides for CO,CH<Subscript>4</Subscript> and NO<Subscript>2</Subscript>

The nanocomplex oxides of Sn-In and Sn-In-Ti were prepared by controlled co-precipitation method as sensing materials of semiconductor gas sensors for detection of CO, CH4 and NO2. Through manipulating the Sn/In cation ratio, metal salt total concentration, precipitation pH value and aging time, the nanocrystalline powders were successfully derived with chemical homogeneity and superior thermal stability, compared with the single component oxides. The particle size and morphology, surface area, and thermal and phase stabilities were characterized using TEM, TG-DTA, BET and XRD. The sensing tests showed that the Sn-In composites exhibit high sensitivity and selectivity for CO and NO2. The introduction of TiO2 enhanced CH4 sensitivity and selectivity, particularly, additives of Pd and Al2O3 as a dopant and surface modification greatly enhanced the sensing properties. The sensitivity depended on the composition of composites, calcination temperature and operating temperature. The optimal values were (25%In2O3- 75%SnO2)-20%TiO2 for ternary composite, 600 and 300℃, respectively. Temperature-programmed desorption (TPD) studies were employed to explain the gas adsorption behavior displayed by the surface of nanocomposites and X-ray photoelectron spectroscopic (XPS) analysis was used to confirm the electronic interactions existing between oxide components. The sensing mechanism of the nanocomposites was attributed to chemical and electronic synergistic effects.     

Microstructure refinement and magnetic properties enhancement of nanocrystalline Nd<Subscript>12.3</Subscript>Fe<Subscript>81.7</Subscript>B<Subscript>6.0</Subscript> ribbons by addition of Zr

Effects of Zr addition and annealing treatment on the formation, microstructure and magnetic properties of Nd_12.3Fe_81.7−x Zr _x B_6.0 (x=0−3.0) ribbons melt-spun and annealed have been systematically investigated by means of vibrating sample magnetometer (VSM), differential scanning calorimeter (DSC), X-ray diffraction (XRD), and high resolution scanning electron microscopy (HRSEM). Phase analysis reveals that Nd₂Fe₁₄B is single-phase material. It has been found that the intrinsic coercivity H _ci of the optimally processed Nd_12.3Fe_81.7−x Zr _x B_6.0 ribbons increases monotonically from 751.7 kA/m for x=0 to 1005.3 kA/m for x=3.0. The remanence polarization J _r and maximum energy product (BH)_max increase first with Zr addition, then slightly decrease with further increasing Zr content. Optimum magnetic properties with J _r=1.041 T, H _ci=887.5 kA/m and (BH)_max=175.2 kJ/m³ have been achieved for the ribbons with x=1.5. The significant improvement of magnetic properties originates from the finer grains of the ribbons by introducing Zr.     

Effect of Fe(III) impurity on the electrochemical performance of LiFePO<Subscript>4</Subscript> prepared by hydrothermal process

Lithium iron phosphate (LiFePO₄) was synthesized from LiOH, FeSO₄ and H₃PO₄ by a hydrothermal process at 180°C. The samples were characterized by X-ray diffraction, scanning electron microscopy and chemical analysis. Electrochemical performance of the samples was tested in terms of charge-discharge capacity and cycling behavior. The results indicated that Fe(III) impurity had obviously effect on the electrochemical properties of LiFePO₄, and the formation of Fe³⁺ was caused by the oxidation of Fe²⁺ in the dissolving and feeding processes accompanying the increase of pH value. It was found that the precipitation separation was effective in decreasing the content of Fe³⁺ in the solution of FeSO₄ and the sealed feeding was useful in preventing the conversion of Fe²⁺ to Fe³⁺. When the content of Fe³⁺ < 0.5 wt%, the hydrothermally synthesized LiFePO₄ calcined at 750°C with sucrose as carbon source exhibited an initial discharge capacity of 154.9 mAh·g⁻¹ at the rate of 0.1 C (1 C = 150 mA·g⁻¹) and the cycling retention rate could reach 98% after 50 cycles at room temperature.     

Fluorescence detection for H<Subscript>2</Subscript>PO<Subscript>4</Subscript><Superscript>-</Superscript> based on carbon dots/Fe<Superscript>3+</Superscript> composite

A novel fluorescent probe for H₂PO₄ ^- was designed and fabricated based on the carbon dots/Fe³⁺ composite. The carbon dots were synthesized by an established one-pot hydrothermal method and characterized by transmission electron microscope, X-ray diffractometer, UV-Vis absorption spectrometer and fluorescence spectrophotometer. The carbon dots/Fe³⁺ composite was obtained by aqueous mixing of carbon dots and FeCl₃, and its fluorescence property was characterized by fluorescence spectrophotometer. The fluorescence of carbon dots was quenched by aqueous Fe³⁺ cations, resulting in the low fluorescence intensity of the carbon dots/Fe³⁺ composite. On the other hand, H₂PO₄ ^- reduced the concentration of Fe³⁺ by chemical reaction and enhanced the fluorescence of the carbon dots/Fe³⁺ composite. The Stern-Volmer equation was introduced to describe the relation between the relative fluorescence intensity of the carbon dots/Fe³⁺ composite and the concentration of H₂PO₄ ^-, and a fine linearity (R ²=0.997) was found in the range of H₂PO₄ ^- concentration of 0.4-12 mM.     

Effect of deposition time on microstructures and growth behavior of ZrC coatings prepared by low pressure chemical vapor deposition with the Br<Subscript>2</Subscript>-Zr-C<Subscript>3</Subscript>H<Subscript>6</Subscript>-H<Subscript>2</Subscript>-Ar System

ZrC coatings were deposited on graphite substrates by low pressure chemical vapor deposition (LPCVD) with the Br₂-Zr-C₃H₆-H₂-Ar system. The effects of deposition time on the microstructures and growth behavior of ZrC coatings were investigated. ZrC coating grew in an island-layer mode. The formation of coating was dominated by the nucleation of ZrC in the initial 20 minutes, and the rapid nucleation generated a fine-grained structure of ZrC coating. When the deposition time was over 30 min, the growth of coating was dominated by that of crystals, giving a column-arranged structure. Energy dispersive X-ray spectroscopy showed that the molar ratio of carbon to zirconium was near 1:1 in ZrC coating, and X-ray photoelectron spectroscopy showed that ZrC was the main phase in coatings, accompanied by about 2.5mol% ZrO₂ minor phase.