Micaceous iron oxide prepared from pyrite cinders by hydrothermal method

Micaceous iron oxide (MIO) with a hexagonal flaky shape was prepared by hydrothermal method. The ferric hydroxide used as precursor was obtained by an acidic leaching solution of pyrite cinders reacting with ammonia solution. The optimal experimental conditions for preparing micaceous iron oxide were investigated by orthogonal experiments. Micaceous iron oxide can be successfully prepared when optimal parameters of total iron concentration of 2.0 mol/L, pH value of 8, n(Fe²⁺)/n(Fe³⁺) of 0.1, mass of seed crystal of 1 g, reaction temperature of 260 °C and reaction time of 30 min are applied. X-ray diffractometry (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and selected area electron diffractometry (SAEM) were adopted to characterize the hydrothermal products prepared under optimal conditions. The results indicate that highly crystallized α-Fe₂O₃ hexagonal flakes, about 1.0–1.5 μm in diameter and 0.1 μm in thickness, are prepared. Furthermore, the quality of micaceous iron oxide prepared can meet the required characteristics of micaceous iron oxide pigments for paints (ISO10601—2007).     

Preparation and characterization of Bi4Ti3O12 platelets by a novel low-temperature molten salt system

Bismuth titanate (Bi₄Ti₃O₁₂) platelets were prepared by molten salt method in a new salt system of CaC_l2-NaCl at 650–750 °C, using bismuth nitrate pentahydrate (Bi(NO₃)₃―H₂O) and titanium butoxide (Ti (OC₄H₉)₄) as raw materials. The synthesis temperature of Bi₄Ti₃O₁₂ platelets was decreased to 650 °C from 900–1100 °C. The phase compositions and crystalline morphology of Bi₄Ti₃O₁₂ platelets were investigated by XRD and SEM. The experimental results indicate that Bi₄Ti₃O₁₂ platelets containing tetragonal and orthorhombic phase with the size of 1–3 μm can be synthesized at 650 °C for 2 h, and the orthorhombic phase becomes the dominant phase at 750 °C for 5 h. The size and proportion of Bi₄Ti₃O₁₂ platelets increase with the increment of the calcining temperature and holding time. The proportion of platelets increases to about ninety percent, and the platelets grow up to about 3–10 μm at 750 °C for 5 h from 1–2 μm at 650 °C for 2 h. This technical route provides a new low-temperature molten salt system for preparing platelets by molten salt methods.     

Iron Fibers Arrays Prepared by Electrodepositing in Reverse Liquid Crystalline

Ordered iron fiber arrays were electrodeposited on the surface of zinc foils using ＂FeSO4 solution-sodium caprylate-Decanol＂ 3-component reverse hexagonal liquid crystal as soft templates. The structure of the soft templates and the synthesized iron ,fibers were characterized by polarizing microscopy, X-ray diffraction （XRD）, scanning electron microscopy （SEM） and energy dispersive X-ray microanalysis etc. The experimental results shou that the synthesized iron fibers with a crystal phase grew up in the form of fiber clusters of about 200 nm along the direction perpendicular to the cathode surface. Each cluster was composed of several tens of fibers. The fibers had almost the same length of more than 10μm with a diameter of about 50 nm.     

Preparation of Ti3SiC2 with Aluminum by Means of Spark Plasma Sintering

Polycrystalline bulk Ti3SiC2 material with a high purity and density was fabricated by spark plasma sintering from the elemental powder mixture with starting composition of Ti3Si3Si1-xAlxC2 , where x = 0. 05 -0.2. X-ray diffraction patterns and scanning electron microscopy photographs of the fully dense samples show that a proper addition of aluminum promotes the formation, and accelerates the crystal growth rate of Ti3SIC2, conse-quently results in a high purity of the prepared samples. The synthesized Ti3 SiC2 is in plane-shape with a size of about 10- 25μm in the elongated dimension. Solid solution of aluminum decreases the thermal stability of Ti3SiC2, and lowers the temperature of Ti3SiC2 decomposeing to be 1300 ℃ .     

Preparation of AgSnO2 composite powders by hydrothermal process

Silver-tin oxide powders were synthesized by the hydrothermal method with Ag（NH3）2^＋ solution and Na2SnO3 solution as raw materials and Na2SO3 as reductant. The precipitation conditions of Na2SnO3 solution and the reduction conditions of Ag（NH3）2^＋ were also investigated. The powders prepared were characterized by differential thermal analysis （DTA）, X-ray diffraction analysis （XRD）, scanning electron microscope （SEM） and energy spectrum analysis, The results show that pH value of the solution is a key parameter in the formation of Sn（OH）4 precipitate and the reduction reaction of Ag（NH3）2^＋ can release H^＋ ions, which results in synchronous precipitation of Sn（OH）6^2- as Sn（OH）4. The reduction of Ag（NH3）2^＋ and precipitation of Na2SnO3 occur simultaneously and the coprecipitation of silver and tin oxide is reached by the hydrothermal method. The silver-tin oxide composite powders have mainly flake shape of about 0.3 μm in thickness and there exists homogeneous distribution of tin oxide and silver in the powder synthesized.     

Valence Control of Ce Ions in Cerium-substituted Yttrium Iron Garnet

Cerium-substituted yttrium iron garnet( CexY3-xFe5O12, Ce : YIG ) was prepared via coprecipitation. The structure, morphology, valence state and constituent of Ce ions were investigated respectively. X-ray powder diffraction( XRD ) analysis shows that Ce : YIG was of single cubic YIG phase. The result of X-ray photoelectron spectroscopy( XPS ) indicates the Ce ions in Ce : YIG were in the state of trivalence. Scanning electron microscope ( SEM ) demonstrates the conglobatian of Ce : YIG particles about 0.2μm scale. The magnetic properties were studied by a vibrating sample magnetometer (VSM) and the result exhibits that substitution of Ce 3 changes the magnetic parameters of YIG. The effects of doping content of Ce ions and synthesis temperature on valence control were discussed in detail.     

Characterization and Electrochemical Properties of LiMn2O4 Thin Films Prepared by Solution Deposition

1 IntroductionThin-filmlithium-ion batteries have attracted greatattention of researchfor possible use inimplantable medi-cal devices , CMOS-based integrated circuits ,radio fre-quency (RF) identification tags for inventory control andanti-theft protection[1],etc. Li Mn2O4thin films , aspromising cathode materials for thin-filmlithium-ion bat-teries, have been prepared by a few methods such aspulsedlaser deposition[2 ,3],electrospraying[4-9],RF mag-netron sputtering[10], laser ablation[11]…     

Effect of tin on the reaction synthesis of ternary carbide Ti3AlC2

The effect of tin on synthesis of Ti₃AlC₂ by spark plasma sintering (SPS) from TiC/Ti/Al powders was investigated. X-ray diffraction (XRD) and scanning electron microscopy (SEM) were used for phase identification and microstructure evaluation. The experimental results show that addition of tin can considerably accelerate the synthesis reaction of Ti₃AlC₂ and fully dense, essentially single-phase polycrystalline Ti₃AlC₂ could be successfully obtained by sintering 2TiC/1Ti/1Al/0.2Sn powders at 1200–1250 °C under a pressure of 30 MPa. SEM images show that Ti₃AlC₂ samples in about 2–5 μm thick and 10–25 μm long platelets can be obtained. The fracture toughness and flexural strength of Ti₃AlC₂ were 6.5±0.2 MPa·m^1/2 and 560±10 MPa, respectively. Funded by the National Natural Science Foundation of China (No.20771088, No.50572080) and Doctoral Foundation of Wuhan University of Technology (No.471-38650142)     

Fabrication of GaN epitaxial films on Al2O3/Si (001) substrates

Single crystal GaN films of hexagonal modification have been fabricated on Al₂O₃/Si (001) substrates via a low pressure metalorganic chemical deposition (LP-MOCVD) method. the full width at half-maximum of (0002) X-ray diffraction peak for the GaN film 1.1 μm thick was 72 arcmin, and the mosaic structure of the film was the main cause of broadening to the X-ray diffraction peak. At room temperature, the photoluminescence (PL) spectrum of GaN exhibited near band edge emission peaking at 365 nm. Project supported by the “863” Advanced materials Committee of China and the Planning Commission of China.     

Preparation of ZrB2 Ceramics by Self-propagating High-temperature Synthesis and Hot Pressing Sintering

ZrB2 ceramics were prepared by self-propagating high-temperature synthesis（SHS） and were sintered by hot pressing（HP）.The effects of the granularities and doses of raw materials in Zr-B2O3-Mgon SHS process and product were investigated.XRD and combustion temperature curves prove that the ideal SHS reactants of Zr-B2O3-Mg are 50μm Zr powder,75μm B2O3 powder and 400μm Mg powder with 45% excessive.The particle sizes of SHS product,acid-leached product,sintered product are 2-5μm,0.5-2μm,2-10μm respectively.Chemical analysis indicates that the acid-leached product consists of ZrB2（94.59%）,ZrO2（3.87%）,and H3BO3（1.54%）,The sintered product has a relative density of 95.4%.     

Fabrication of inorganic film gratings and study on their diffraction properties

A novel process for fabricating high-density and high diffraction efficiency inorganic gratings has been proposed by combining laser interference and chemical etching. In the present work, UV photosensitive Zr-contained sol was synthesized, and photosensitive ZrO₂/BzAc gel films on (100) silicon were prepared using the sol-gel method. Subsequently, inorganic film gratings with a pitch of 1 μm were fabricated by laser interference in this photosensitive gel film combining with the process of heat treatment. In order to increase the depth-to-width ratio of the gratings, chemical etching was adopted by using iodine-saturated KOH as anisotropic etchant, which improved the diffraction efficiency of the gratings effectively. Furthermore, the diffraction efficiency was improved by gold coating to enhance the surface glossiness and reflection coefficient. Supported by the National Natural Science Foundation of China (Grant No. 90401009) and the Xi’an Applied Materials Innovation Fund (Grant No. XA-AM-200611)     

Preparation of Bauxite Ceramic Microsphere

Ceramic microspheres were prepared by using Chinese bauxite as raw materials through the centrifugal spray drying method. The control technology of microsphere size, degree of sphericity was researched. The ceramic microspheres were sintered by a double sintering process. The microstructure and composition of ceramic microsphere were investigated by X-ray diffraction （XRD）, scanning electron microscopy （SEM） and X-ray energy spectroscopy. The results show that the degree of sphericity of the ceramic microsphere was good and the particle size was 10-100 μm. The XRD analysis reveals that the main crystalline phase of the ceramic microsphere was a-Al2O3 and mullite （3Al2O3·2SiO2）. The product can be used as reinforced material for composite material, especially for antiskid and hard wearing aluminum alloy coating.     

Effect of acetic acid on electrochemical deposition of carbon-nitride thin film

Electrochemical deposition method was employed to prepare CNx thin film from methanol-urea solution,and it was shown that adding a little acetic acid in the solution significantly affected the deposition process.After optimizing the experiment conditions,we obtained polycrystalline grains with sizes of about 3―7μm on the faces of single crystal silicon.X-ray diffraction spectrua indicate that the grains are mainly composed of cubic phase mixed with a small amount of β and α phases.     

Controlled synthesis and magnetic properties of Fe<Subscript>3</Subscript>O<Subscript>4</Subscript> walnut spherical particles and octahedral microcrystals

Magnetite Fe₃O₄ walnut spherical particles and octahedral microcrystals were successfully synthesized from K₄ [Fe (CN)₆], K₃ [Fe (CN)₆] and NaOH reagents via a simple hydrothermal process. And the uniform morphology of octahedral microcrystals was obtained in the presence of ethylene glycol. The morphology and structure of products were characterized by powder X-ray diffraction, scanning electron microscopy and transmission electron microscopy. The results showed that the Fe₃O₄ walnut spherical particles and octahedral microcrystals were single crystals with the face-center cubic structure and with size distributions from 2.2 to 8.6 μm and 1.6 to 12.5 μm, respectively. Their magnetic properties were detected by a vibrating sample magnetometer at room temperature. The walnut spherical particles exhibited a ferromagnetic behavior with the coercive force (Hc), saturation magnetization (Ms) and remanent magnetization (Mr) being 150.57 Oe, 97.634 and 12.05 emu/g, respectively. For the octahedral microcrystals they were 75.28 Oe, 101.90 and 6.69 emu/g, respectively. Different sizes of walnut spherical particles were controlled synthesized through adjusting the NaOH concentration. It was found that ethylene glycol molecules have a significant effect on the formation of Fe₃O₄ octahedra. A possible mechanism was also proposed to account for the growth of these Fe₃O₄ products. Supported by Fund of weinan Teachers University (Grant No. 08YKZ008), the National Natural Science Foundation of China (Grant No. 20573072) and Doctoral Fund of Ministry of Education of China (Grant No. 20060718010)     

Photocatalytic H2 evolution activity of CuO/ZrO2 composite catalyst under simulated sunlight irradiation

Zirconia-supported CuO (CuO/ZrO₂) composite photocatalysts were successfully synthesized via citric acid-assisted sol-gel technique. For comparison, CuO/ZrO₂ materials were also prepared by solid state reaction and co-precipitation method. The as-prepared powders were characterized by X-ray diffractometry (XRD), transmission electron microscopy (TEM), and thermogravimetric-differential thermal analysis (TG-DTA). The photocatalytic activity of CuO/ZrO₂ catalyst was investigated based on the H₂ evolution from oxalic acid solution under simulated sunlight irradiation. The effects of molar ratio of CuO to ZrO₂, preparation method, phase change with the calcination temperature and the durability on the photocatalytic activity of the photocatalyst were investigated in detail. It is found that the optimal activity of photocatalytic H₂ evolution (2.41 mmol·h⁻¹μ⁻¹) can be obtained when CuO/ZrO₂ composite photocatalyst is synthesized by sol-gel technique and the mole ratio of CuO to ZrO₂ is 40%. The activity of copper oxide supported on monoclinic ZrO₂ calcined at higher temperature is much higher than that on tetragonal ZrO₂ calcined at lower temperature, and the best calcination temperature is 900 °C.     

Local segregation in Cu-In precursors and its effects on microstructures of selenized CuInSe2 thin films

Local segregation in Cu-In precursors and its effects on the element distribution and microstructures of selenized CuInSe₂ thin films were investigated. Cu-In precursors with an ideal total mole ratio of Cu to In of 0.92 were prepared by middle frequency alternating current magnetron sputtering with Cu-In alloy target, then CuInSe₂ absorbers for solar cells were formed by selenization process in selenium atmosphere. Scanning electron microscope and energy dispersive X-ray spectroscope were used respectively to observe the surface morphologies and determine the compositions of both Cu-In precursors and CuInSe₂ thin films. Their microstructures were characterized by X-ray diffractometry and Raman spectroscope. The results show that Cu-In precursors are mainly composed of Cu₁₁In₉ phase with In-rich solid solution. Stoichiometric CuInSe₂ thin films with a homogeneous element distribution and single chalcopyrite phase can be synthesized from a segregated Cu-In precursor film with an ideal total mole ratio of Cu to In of 0.92. CuInSe₂ thin film shows P-type conductivity and its resistivity reaches 1.2×10³ Θ·cm. Foundation item: Project(2004AA513023) supported by the National High Technology Research and Development Program of China     

Effects of heat treatment temperature on crystallization and thermal expansion coefficient of Li2O-Al2O3-SiO2

The basic glass of Li₂O-Al₂O₃-SiO₂ system using P₂O₅ as nucleator was prepared by means of conventional melt quenching technology, and the heat-treatment process was determined by using differential thermal analysis. The crystalline phases and the microstructure of the glass-ceramics were investigated by using X-ray diffraction and scanning electron microscopy. The results show that the glass based on Li₂O-Al₂O₃-SiO₂ oxides using P₂O₅ as nucleator can be prepared at lower melt temperature of 1450°C and the glass-ceramics with lower thermal expansion coefficient of 21.6 × 10⁻⁷°C⁻¹ can also be obtained at 750°C. The glass-ceramics contain a few crystal phases in which the main crystal phase is β-quartz solid solution and the second crystal phase is β-spodumene solid solution. When the heat treatment temperature is not higher than 650°C, the transparent glass-ceramics containing β-quartz solid solution can be prepared. β-quartz solid solution changes into β-spodumene solid solution at about 750°C. And the appearance of the glass-ceramics changes from translucent, part opaque to complete opaque with increasing temperature.     

Synthesis of Magnetic Manganese Ferrite

MnFe2O4 polycrystalline powders were prepared by the chemical coprecipitation method. When the reaction temperature is above 80 ℃, through depositing and washing, the MnFe2O4 can be obtained directly without calcining. However, when it is below 80 ℃, we have to calcine the precursor in order to obtain MnFe2O4, which does not result in pure spinal structure but a mixture of MnFe2O4 and α-Fe2O3. The powders＇ magnetic property was characterized with a Vibrating Sample Magnetometer. The phase structure, crystal size and lattice constant were presented by an X-ray diffractometer. In addition, the morphology of the powder was observed with a scan electron microscope and a transmission electron microscope.     

Preparation of basic magnesium carbonate and its thermal decomposition kinetics in air

The thermal decomposition process of basic magnesium carbonate was investigated. Firstly, Basic magnesium carbonate was prepared from magnesite, and the characteristics of the product were detected by X-ray diffraction (XRD) and scanning electron microscopy (SEM). Subsequently, the thermal decomposition process of basic magnesium carbonate in air was studied by thermogravimetry-differential thermogravimetry (TG-DTG). The results of XRD confirm that the chemical composition of basic magnesium carbonate is 4MgCO₃·Mg(OH)₂·4H₂O. And the SEM images show that the sample is in sheet structure, with a diameter of 0.1–1 μm. The TG-DTG results demonstrate that there are two steps in the thermal decomposition process of basic magnesium carbonate. The apparent activation energies (E) were calculated by Flynn-Wall-Ozawa method. It is obtained from Coats-Redfern’s equation and Malek method that the mechanism functions of the two decomposition stages are D3 and A1.5, respectively. And then, the kinetic equations of the two steps were deduced as well.     

Synthesis and structural characterization of macroporous bioactive glass

Porous sol-gel glass of CaO-SiO2-P2O5 system with macropores larger than 100 μm was prepared by adding stearic acid as pore former when the sintering was carried out at 700 ℃ for 3 h. The sol-gel porous glass shows an amorphous structure. The diameter of the pore created by pore former varies from 100 to 300 μm, and macroporous glass has a narrow and small pore size distribution in mesoporous scale. The porosity and pore size ofmacroporous bioactive glass can be controlled.