Corrosion resistance of plasma sprayed NiCrAl+(ZrO2+Y2O3) thermal barrier coating on 18-8 steel surface

The corrosion resistance of NiCrAl+(ZrO₂+Y₂O₃) thermal barrier coating, formed with the plasma spraying technique, on the 18 - 8 steel surface was investigated. The phase structure and morphology of the coating were analyzed by means of X-ray diffraction (XRD) and scanning electron microscopy (SEM). The electrochemical corrosion behavior of the coating in 1.0 mol/L H₂SO₄ solution was studied by using electrochemical measurement methods. The results show that the gradient plasma spraying coating is composed of the NiCrAlY coating and the (ZrO₂+Y₂O₃) top coating, and the coating thickness is 360 μm. The microhardness of coating reaches 1 100 HV. The corrosion resistance of the plasma sprayed coating of the 18 - 8 steel surface is about 5 times as great as that of the original pattern. The corrosion resistance of the coating is enhanced notably. Foundation item: Project (5040202140) supported by Scientific Research Common Program of Beijing Municipal Commission of Education     

Synthesis and characterization of (PEO)<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>−(V<Subscript>0.85</Subscript>Mo<Subscript>0.15</Subscript>)<Subscript>2</Subscript>O<Subscript>5</Subscript> nanocomposite films

(PEO) _x −(V_0.85Mo_0.15)₂O₅(x=0,0.5,1.0) nanocomposite films were prepared by a modified sol-gel method. The structure of the films was analyzed by XRD, and the DC electrical conductivity. Cyclic voltammogram and optical spectral transmittance were investigated. The results show that the (V_0.85Mo_0.15)₂O₅ xerogel has a layered structure and its interlayer space increased from 1.3181 nm at x=0 to 1.7897 nm at x=1.0. The introduction of MoO₃ improved the DC electrical conductivities of the films due to the generation of V₄₊ to maintain the electrical neutrality of the oxides. PEO intercalated in the interlayer of (V_0.85Mo_0.15)₂O₅ oxides has interaction with the oxides, enhancing the amount of Li⁺ ions inserted into the interlayer of the oxides. Moreover, the intercalation of PEO into the interlayer of (V_0.85Mo_0.15)₂O₅ oxides improved the cathodic electrochromic property in near ultraviolet region and anodic electrochromic property in visible range. JIANG Cong-sheng: Born in 1963 Supported by the Science Foundation of Hubei Province (Grant No. 2001ABB083)     

Preparation and electrochemical studies of Y-doped LiVPO<Subscript>4</Subscript>F cathode materials for lithium-ion batteries

Y-doped LiVPO₄F cathode materials were prepared by a carbothermal reduction(CTR) process. The properties of the Y-doped LiVPO₄F samples were investigated by X-ray diffraction (XRD) and electrochemical measurements. XRD studies show that the Y-doped LiVPO₄F samples have the same triclinic structure as the undoped LiVPO₄F. The Li extraction/insertion performances of Y-doped LiVPO₄F samples were investigated through charge/discharge, cyclic voltammogram (CV), and electrochemical impedance spectra(EIS). The optimal doping content of Y is x=0.04 in LiY _x V_1−x PO₄F system. The Y-doped LiVPO₄F samples show a better cyclic ability. The electrode reaction reversibility is enhanced, and the charge transfer resistance is decreased through the Y-doping. The improved electrochemical performances of the Y-doped LiVPO₄F cathode materials are attributed to the addition of Y³⁺ ion by stabilizing the triclinic structure. Funded by the Sponsor Teams for Innovation in the Construction of Talent Highlands in Guangxi Institutions of Higher Learning(GuiJiaoRen [2007]71), Guangxi Natural Science Foundation(No.0832259), the Research Funds of the Guangxi Key Laboratory of Environmental Engineering, Protection and Assessment Program to Sponsor Teams for Innovation in the Construction of Talent Highlands in Guangxi Institutions of Higher Learning(GuiJiaoRen [2007]71)     

In situ prepared Al-Si alloy matrix composites reinforced by γ-Al2O3p

A γ-Al2O3 particles reinforced Al-Si alloy matrix composite was fabricated by adding NH4Al（SO4）2 to molten aluminum alloy. TEM observation shows that in-situ γ-Al2O3 particles are generally spherical and uniformly distributed in the matrix. The results of dry sliding wear tests show that the wear resistance of the composites increases with increasing mass fraction, and the volume loss is considerably lesser than that of the matrix and is lesser than that of the composites by adding γ-Al2O3 particles directly.     

Synthesis and photoluminescence property of red phosphors LiEu1?xYx(WO4)0.5(MoO4)1.5 for white LED

A series of novel red phosphors LiEu_1−x Y _x (WO₄)_0.5(MoO₄)_1.5 (x=0, 0.1, 0.2, 0.3, 0.4, 0.5, 0.6, 0.8) were synthesized by conventional solid state reaction method with the starting materials: WO₃, MoO₃, Eu₂O₃, Li₂CO₃ and Y₂O₃. The spectrum and the crystal structure of the phosphors were characterized by F-4500 and XRD respectively. Meanwhile the effects of flux and Y³⁺ concentration on the crystal structure and luminescent properties of the phosphors were investigated. The results showed that the optimal content of flux () was 1 wt% and the optimal doping concentration of Y³⁺ was 0.5 mol. The emission spectrum showed the most intense peak was located at 615 nm, which corresponds to the ⁵ D ₀→⁷ F ₂ transition of Eu³⁺ and that Eu³⁺ occupied the lattice site of noncentrosymmetric environment in the scheelite phases. The excitation spectrum displayed that these phosphors could be effectively excited by ultraviolet (UV) (396 nm) and blue (466 nm) light, nicely in correspondence with the widely applied output wavelengths of ultraviolet or blue LED chips. The influence of flux on the luminescent properties of LiEu_0.5Y_0.5(WO₄)_0.5(MoO₄)_1.5 phosphor was analyzed. The XRD spectra indicated that the flux could help to crystallize the phosphor, and no other phases were formed except the tetragonal. When adding flux, the relative intensity of LiEu_0.5Y_0.5(WO₄)_0.5(MoO₄)_1.5 became much stronger and the average particle size of the phosphor decreased. Supported by the Key Programs for Science and Technology Development of Hubei Province (Grant No. 2005AA105A05)     

Molten salts/ceramic-foam matrix composites by melt infiltration method as energy storage material

A new type of high temperature energy storage material was obtained through the melt infiltration method, using compounding SiC ceramic foam as matrix and Na₂SO₄ as phase change material. The resulting composite material was measured by XRD, SEM, TG-DSC methods. The experimental results indicate that the composite is composed of silicon carbide, sodium sulfate and square quartz, and no chemical reactions occurs between Na₂SO₄ and SiC matrix. Na₂SO₄ has a good bonding with the SiC ceramic foam matrix. As the composite material is characterized by high thermal energy storage density and high thermal conductivity, it is suit for energy storage under high temperature. Funded by the “863” Hi-Tech Research and Development Program of China (2008AA05Z418)     

Molar heat capacities of La2Mo2O9 and La1.9Sr0.1MO209-δ

The molar heat capacities of La2Mo209 and La1.9Sr0.1MO209-δ were obtained using the differential scanning calorimetry （DSC） technique in a temperature range from 298 to 1473 K. The DSC curve of La2Mo209 showed an endothermal peak around 834 K corresponding to a first-order monoclinic-cubic phase transition, and the enthalpy change accompanying this phase transition is 5.99 kJ/mol. No evident endothermal peak existed in the DSC curve of La1.9Sr0.1MO209-δ, but a broad thermal anomaly existed in its heat capacity curve at around 832 K. In addition, the heat capacity values of La2Mo209 and La1.9Sr0.1MO209-δ began to decrease at 1196 and 1330 K, respectively. The non-transitional heat capacity values of La2Mo209 and La1.9Sr0.1MO209-δ were formulated using multiple regression analysis in two temperature ranges.     

Self-Propagating High-Temperature Reduetive Synthesis of TiB2-Al2O3 Composite Powders

TiB2-Al2O3 composite powders were produced by self-propagating high-temperature synthesis（SHS） method with reductive process from B2O3-TiO2-AI system. X-ray diffraction（XRD） and scanning electron microscopy（SEM） analyses show the presence of TiB2 and Al2O3 only in the composite powders produced by SHS. The powders are uniform and free-agglomerate. Transmission electron microscopy （TEM） and high resolution electron microscopy （HREM） observation of microstructure of the composite powders indicate that the interfaces of the TiB2-Al2O3 bond well, without any interfacial reaction products. It is proposed that the good interfacial bonding of the composite powders can be resulted from the TiB2 particles crystallizing and growing on the Al2O3 particles surface with surface defects acting as nucleation centers.     

Recovery of copper sulfate after treating As-containing wastewater by precipitation method

The solid sodium hydroxide neutralized acidic As-containing wastewater till pH value was 6. Green copper arsenite was prepared after copper sulfate was added into the neutralized wastewater when the molar ratio of Cu to As was 2:1 and pH value of the neutralized wastewater was adjusted to 8.0 by sodium hydroxide. The arsenious acid solution and red residue were produced after copper arsenite mixed with water according to the ratio of liquid to solid of 4:1 and copper arsenite was reduced by SO₂ at 60 °C for 1 h. The white powder was gained after the arsenious acid solution was evaporated and cooled. Copper sulfate solution was obtained after the red residue was leached by H₂SO₄ solution under the action of air. The results show that red residue is Cu₃(SO₃)₂·2H₂O and the white powder is As₂O₃. The leaching rate of Cu reaches 99.00% when the leaching time is 1.5 h, molar ratio of H₂SO₄ to Cu is 1.70, H₂SO₄ concentration is 24% and the leaching temperature is 80 °C. The direct recovery rate of copper sulfate is 79.11% and the content of CuSO₄·5H₂O is up to 98.33% in the product after evaporating and cooling the copper sulfate solution.     

Microstructures and mechanism of Al<Subscript>2</Subscript>O<Subscript>3</Subscript>/Al composites fabricated by the reaction between SiO<Subscript>2</Subscript> and molten aluminum

Al₂ O₃/Al composite was fabricated by the reaction between SiO₂ and molten aluminum. The microstructures of the composite obtained under different reaction conditions were analyzed. The formation mechanism of the composite microstructure was discussed. Results show that the reaction kinetics is influenced remarkably by the reaction temperature, reaction time and the quantity of SiO₂. The morphologies of Al₂O₃ have different features, depending on the reaction temperature. The composite has equaxed Al₂O₃ grains when materials reacted below 1200°C, and the composite is composed of a large number of fine Al₂O₃ grains and aluninum. The composite has a frame-shaped Al₂O₃ microstructure at the reaction temperature of above 1250°C. CHENG Xiao-min: Born in 1964 Funded by the National Natural Science Foundation of China (No. 91522)     

Preparation of LiFePO4 for lithium ion battery using Fe2P2O7 as precursor

In order to obtain a new precursor for LiFePO4, Fe2P2O7 with high purity was prepared through solid phase reaction at 650 ℃ using starting materials of FeC2O4 and NH4H2PO4 in an argon atmosphere. Using the as-prepared Fe2P2O7, Li2CO3 and glucose as raw materials, pure LiFePO4 and LiFePO4/C composite materials were respectively synthesized by solid state reaction at 700 ℃ in an argon atmosphere. X-ray diffractometry and scanning electron microscopy（SEM） were employed to characterize the as-prepared Fe2P2O7, LiFePO4 and LiFePO4/C. The as-prepared Fe2P2O7 crystallizes in the Cl space group and belongs to β-Fe2P2O7 for crystal phase. The particle size distribution of Fe2P2O7 observed by SEM is 0.4-3.0 μm. During the Li^＋ ion chemical intercalation, radical P2O7^4- is disrupted into two PO4^3- ions in the presence of O^2-, thus providing a feasible technique to dispose this poor dissolvable pyrophosphate. LiFePO4/C composite exhibits initial charge and discharge capacities of 154 and 132 mA·h/g, respectively.     

球形LiMn1.5Ni0.5O4材料的嵌脱动力学

为明晰Li Mn1.5Ni0.5O4正极材料的动力学性能,采用水热辅助共沉淀法合成了尖晶石Li Mn1.5Ni0.5O4正极材料,并采用扫描电镜(SEM)、X射线粉末衍射(XRD)和电化学阻抗(EIS)研究了材料的结构和锂离子嵌脱动力学.实验结果表明:共沉淀法制备的Li Ni0.5Mn1.5O4材料颗粒呈均匀球形,且平均粒径较小,粒度分布较窄.在循环过程中,Li Ni0.5Mn1.5O4的电荷转移电阻增大,锂离子扩散系数减小,进而电子电导率和离子电导率下降.温度升高后,Li Ni0.5Mn1.5O4材料的溶液电阻变化不大,但是电荷转移电阻逐渐增大,锂离子扩散系数逐渐减小;此外,随着温度的升高,Li Ni0.5Mn1.5O4材料的溶解速度加快,从而导致SEI膜的厚度增大.Li Ni0.5Mn1.5O4材料的嵌脱锂动力学与温度和循环次数有密切关系.     

Fabrication and characterization of composite YSZ-La9.33Si6O26 oxygen-ion conductor

To improve the conductivity of Y₂O₃-stabilized ZrO₂ (YSZ) based oxygen-ion conductor, Zr_0.85Y_0.15O_1.925-La_9.33Si₆O₂₆ (YSZ-LSO) composite ceramics with the mass fraction of La_9.33Si₆O₂₆ (LSO) of 15% were prepared by using a modified coprecipitation method. The phases, microstructures and conductivities of the YSZ, LSO and YSZ-LSO were investigated by X-ray diffraction, electron microscopy and complex impedance, respectively. The results show that the as-calcined powder of YSZ-LSO composite has the grain size less than 10 nm, and the as-sintered composite ceramics are composed of YSZ and LSO phases. The conductivity can be enhanced obviously by composite method. At 700 °C, the conductivity of the composite ceramic is 0.125 S/cm, which is one order in magnitude higher than that of the YSZ ceramic and two orders in magnitude higher than that of LSO ceramic. By analyzing the impedance spectra and modulus spectra, the interfacial effect on the conductivity improvement was proposed.     

Preparation and properties of 4.25Cu-0.75Ni／NiFe2O4 cermet

4.25Cu-0.75Ni/NiFe₂O₄ cermets were prepared by doping NiFe₂O₄ ceramic matrix with the mixed powders of Cu and Ni or Cu-Ni alloy powder as the electrical conducting metallic elements. The effects of technological parameters, such as the adding modes of metallic elements, the ball milling time, the sintering time and the sintering temperature, on the relative density and resistivity of the cermets were studied. The results show that the resistivity of 4.25Cu-0.75Ni/NiFe₂O₄ cermets decreases with increasing temperature, and has a turning point at 590 °C, which is similar to that of NiFe₂O₄ ceramic. The sintering temperature and adding modes of metallic elements have a great influence on the properties of 4.25Cu-0.75Ni/NiFe₂O₄ cermets. When the sintering temperature increases from 1200 °C to 1300 °C, the relative density increases from 89.86% to 95.33%, and the resistivity at 960 °C decreases from 0.11 Ω · cm to 0.03 Ω · cm, respectively. When the metallic elements are added with the mixed powders of Cu and Ni, the cermets of finely and uniformly dispersed metallic phase, high density and electric conductivity are obtained. The relative density and resistivity at 960 °C are 90.23% and 0.04 Ω · cm respectively for the cermet samples sintered at 1200 °C for 2 h, which are both better than those of the cermets prepared under the same technique conditions but with the metallic elements added as 85Cu-15Ni alloy powders. Foundation item: Project (G1999064903) supported by the National Key Fundamental Research and Development Program of China; project(2001AA335013) supported by the National High Technology Research and Development Program of China; project (50204014) supported by the National Natural Science Foundation of China     

Properties of plasma sprayed NiCrAlY+(ZrO2+Y2O3) coating on refractory steel surface

NiCrAlY+(ZrO₂+Y₂O₃) thermal barrier coating was prepared on the surface of refractory steel 1Cr18Ni9Ti with plasma spraying technique. The phases and microstructure of the thermal barrier coating were determined by scanning electron microscopy (SEM) and X-ray diffraction (XRD). The results show that the bonding between thermal barrier coating and substrate is sound. The surface hardness of 1Cr18Ni9Ti reaches up to 1 000 HV, but that of substrate is only 300 HV. The patterns sprayed with CoNiCrAlY+(ZrO₂+Y₂O₃) ceramic coating have a good heat insulation effect at 800 °C for heat insulation temperature difference reaches 54 °C, which increases the operating temperature and service life of refractory steel. Foundation item: Project (5040202140) supported by Scientific Research Common Program of Beijing Municipal Commission of Education     

Preparation of λ-MnO2 by Column Method and Its Ion-Sieve Property

λ-MnO₂ was prepared by column method from normal spinel LiMn₂O₄ with purity of 99.38%. The influence of LiMn₂O₄ grain size and acidity of leaching solution on the lithium leaching process was studied. The results show that the appropriate range of LiMn₂O₄ grain size was 60–160 meshes and the concentration of leaching solution HCl was 0.1 mol·L⁻¹. The adsorption capacity Q of λ-MnO₂ for lithium increased with the increase of pH and changed markedly at pH 6.0–10.0. It was 3.80mmol/g at pH 12.0 The distribution coefficients K_d of Li⁺ and Na⁺ were 3.406×10⁴ and 2.300 respectively, and the separation coefficient a _Na ^Li was 1.481 ×10⁴ at pH 6.5. As a result, λ-MnO₂ is a high performance ion-sieve material for lithium ion. LEI Jia-heng: Born in 1957. Funded by the National Natural Science Foundation of China (No. 59972027) and the Natural Science Foundation of Hubei Province (No. 2002AB074)).     

Effects of CFB Ash on the Adsorption Mechanism of Polycarboxylate Superplasticiser

The effects of circulating fluid bed(CFB) ash on the adsorption performance of polycarboxylate superplasticiser and the mechanism of this influence on the dispersive property of the polycarboxylate superplasticiser were investigated by determing the cement paste fluidity, total organic carbon adsorption, infrared spectroscopic analyses and ζ potential test. The experimental results show that the addition of an inorganic salt into the mixture to change the content of SO_4~(2-)and Fe_2 O_3 can improve the adaptability between the CFB ash and polycarboxylate superplasticiser. Adsorption may occur between the polycarboxylate superplasiciser and Fe_2 O_3, SO_4~(2-)or other components in CFB ash, leading to a significant reduction in paste fluidity. As the content of Na_2 SO_4 in CFB ash reaches 3% or Fe_2 O_3 reaches 9%, the paste loses its liquidity. The organic carbon content in the liquor decreases with an increase in Na2_ SO_4 or Fe_2 O_3 content. Adding some Ba(NO_3)_2 and Na_2 S to the liquor can recover the organic carbon content to a certain extent, and the absolute value of ζ potential will increase. The addition of Ba(-NO_3)_2 or Na_2 S reduces the adsorption property of Na_2 SO_4 or Fe_2 O_3 in CFB ash on the polycarboxylate superplasticiser.     

Valence electron structure and properties of stabilized ZrO2

To reveal the properties of stabilizers in ZrO₂ on nanoscopic levels, the valence electron structures of four stable ZrO₂ phases and c-ZrO₂ were analyzed on the basis of the empirical electron theory of solids and molecules. The results showed that the hybridization levels of Zr atoms in c-ZrO₂ doped with Ca and Mg dropped from B17 to B13, the hybridization levels of Zr atoms in c-ZrO₂ doped with Y and Ce dropped from B17 to B15, and that the four stabilizing atoms all made the hybridization levels of O atoms drop from level 4 to level 2. The numbers of covalent electrons in the strongest covalent bond in the descending order are c-ZrO₂>Zr_0.82Ce_0.18O₂>Zr_0.82Y_0.18O_1.91>Zr_0.82Mg_0.18O_1.82>Zr_0.82Ca_0.18O_1.82. The bond energies of the strongest covalent bond and the melting points of the solid solutions in the descending order are Zr_0.82Ce_0.18O₂> c-ZrO₂>Zr_0.82Y_0.18O_1.91>Zr_0.82Mg_0.18O_1.82>Zr_0.82Ca_0.18O_1.82. The percentages of the total number of covalent electrons in the descending order are c-ZrO₂>Zr_0.82Y_0.18O_1.91> Zr_0.82Ce_0.18O₂>Zr_0.82Mg_0.18O_1.82> Zr_0.82Ca_0.18O_1.82. From the above analysis, it can be concluded that the stabilizing degrees of the four stabilizers in the descending order are CaO> MgO>Y₂O₃>CeO₂. Supported by the Major Project of the National Natural Science Foundation of China (Grant No. 90505015)     

Preparation of uitrafine α-Al2O3 powders by catalytic sintering of ammonium aluminum carbonate hydroxide at low temperature

The precursor of ammonium aluminum carbonate hydroxide was synthesized by using aluminum sulfate （Al2 （SO4）3 ） and ammonium carbonate（（NH4 ）2CO3 ）. The effects of α-Al2 O3 seeds and mixture composed of α- Al2O3 and ammonium nitrate, as well as multiplex catalysts （AT） on phase transformation of alumina in sintering process were investigated respectively. The results show that the α-Al2 O3 seeds and the mixture of α-Al2 O3 and ammonium nitrate can lower the phase transformation temperature of α-Al2O3 to different extents while the particles obtained agglomerate heavily. AT has great potential synergistic effects on the phase transformation of alumina and reduces the phase transformation temperature of α-Al2O3 and the trends of necking-formation between particles. Therefore the dispersion of powder particles is improved significantly.     

Characteristics of LiCoO2, LiMn2O4 and LiNi0.45Co0.1Mn0.45O2 as cathodes of lithium ion batteries

LiNi_0.45Co_0.10Mn_0.45O₂ was synthesized from Li₂CO₃ and a triple oxide of nickel, cobalt and manganese at 950 °C in air. The structures and characteristics of LiNi_0.45Co_0.10Mn_0.45O₂, LiCoO₂ and LiMn₂O₄ were investigated by XRD, SEM and electrochemical measurements. The results show that LiNi_0.45Co_0.10Mn_0.45O₂ has a layered structure with hexagonal lattice. The commercial LiCoO₂ has sphere-like appearance and smooth surfaces, while the LiMn₂O₄ and LiNi_0.45Co_0.10Mn_0.45O₂ consist of cornered and uneven particles. LiNi_0.45Co_0.10Mn_0.45O₂ has a large discharge capacity of 140.9 mA · h/g in practical lithium ion battery, which is 33.4% and 2.8% above that of LiMn₂O₄ and LiCoO₂, respectively. LiCoO₂ and LiMn₂O₄ have higher discharge voltage and better rate-capability than LiNi_0.45Co_0.10Mn_0.45O₂. All the three cathodes have excellent cycling performance with capacity retention of above 89.3% at the 250th cycle. Batteries with LiMn₂O₄ or LiNi_0.45Co_0.10Mn_0.45O₂ cathodes show better safety performance under abusive conditions than those with LiCoO₂ cathodes. Foundation item: Project(50302016) supported by the National Natural Science Foundation of China; Project(2005037698) supported by the Postdoctoral Science Foundation of China