Coating of Fe, Ni on α-alumina microspheres by heterogeneous precipitation

1INTRODUCTION Themagneticmetal coatedceramicoxides,core shellstructuralcompositematerials,inwhichthinmetallicfilmsarecoatedonaceramicoxide matrixwithmicrometerparticlesizes,areattrac tiveduetothecombinationofthefunctionalchar acteristicsofmetalsandmechanicalpropertiesoftheceramicmatrix.Theceramic basedtransition metal coated,core shellcompositessuchasNi coatedAl2O3[1],Fe coatedAl2O3[2],FeNi coated Al2O3[3]orCoFe coatedSiO2[4],havebeenfoundtoexhibitinterestingfunctionalperformancesdue…     

Thermal Behavior Study of Carbonate Inorganic Materials

The thermal decomposition processes of(MgCO_3)_4·Mg(OH)_2·5H_2O(MCH),5ZnO·2CO_3·4H_2O(ZCH),NiCO_3·2Ni(OH)_2·4H_2O(NCH),PbCO_3(LC)and [Cr(OH)_5]_2·CO_3·8H_2O(CC)were studied via TG-DSC.The results of research imply that MCH has the largest capacity of heat absorption and ZCH is second to MCH among the studied materials.The non-isothermal kinetic parameters of MCH and ZCH were calculated by Kissinger and Ozawa methods.Furthermore,thermal decomposition mechanisms of MCH and ZCH were investigated by Coats-Redfern method.Due to the large specific heat capacity,MCH and ZCH are promising to be used as a coolant in extinguishant formulations.     

Mg<Subscript>2</Subscript>(OH)<Subscript>2</Subscript>CO<Subscript>3</Subscript>·3H<Subscript>2</Subscript>O whiskers growth mechanism

From the perspective of growth units, the growth mechanism of Mg₂(OH)₂CO₃·3H₂O whisker is investigated in this paper. Results show that the growth morphology of Mg₂(OH)₂CO₃·3H₂O whisker is consistent with the model of anion coordination polyhedron growth units. The growth solution Raman shift of Mg₂(OH)₂CO₃·3H₂O was monitored using Raman spectroscopy. The growth units are [Mg-(OH)₄]^2- and H₂CO₃. The growth process of Mg₂(OH)₂CO₃·3H₂O whisker is as follows: growth unit [Mg-(OH)₄]^2- first incorporates into the larger dimension [Mg-(OH)₄] _n ^2- , then the [Mg-(OH)₄] _n ^2- combines with H₂CO₃ into a linear skeleton Mg₂(OH)₂CO₃ in the same line. Mg₂(OH)₂CO₃ combines with H₂O by hydrogen bonds and ultimately transforms into Mg₂(OH)₂CO₃·3H₂O whisker. Magnesium carbonate whiskers have a layered structure, each of which is made of magnesium, carbon, oxygen, with H₂O in between each layer. When skeletons are superimposed within the same plane as a parallelepiped one, they grow into solid cuboid-shaped whiskers. When the parallelepiped skeletons planes combine with each other through the cascading links, they grow into hollow cylindrical whiskers.     

Preparation and electrochemical properties of Co3O4/graphite composites as anodes of lithium ion batteries

Co₃O₄/graphite composites were synthesized by precipitation of cobalt oxalate on the surface of graphite and pyrolysis of the precipitate, and the effects of graphite content and calcination temperature on the electrochemical properties of the composites were investigated. The samples were characterized by thermogravimetry and differential thermal analysis (TG/DTA), X-ray diffractometry (XRD), scanning electron microscopy (SEM), cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS) and charge/discharge measurements. With increasing the graphite content, the reversible capacity of the Co₃O₄/graphite composites decreases, while cycling stability improves dramatically, and the addition of graphite obviously decreases the average potential of lithium intercalation/deintercalation. The reversible capacity of the composites with 50% graphite rises from 583 to 725 mA·h/g as the calcination temperature increases from 300 to 500 °C, and the Co₃O₄/graphite composites synthesized at 400 °C show the best cycling stability without capacity loss in the initial 20 cycles. The CV profile of the composite presents two couples of redox peaks, corresponding to the lithium intercalaction/deintercalation for graphite and Co₃O₄, respectively. EIS studies indicate that the electrochemical impedance decreases with increasing the graphite content.     

Two-step synthesis of TiC<Subscript>0.7</Subscript>N<Subscript>0.3</Subscript>@WC-MoC<Subscript>2</Subscript> core-shell microspheres and fabrication of TiC<Subscript>0.7</Subscript>N<Subscript>0.3</Subscript>@WC-MoC<Subscript>2</Subscript>-based cermets by SPS

The precursor with TiC0.7N0.3@WO3-MO3 microspheres were prepared by a novel method from the WO3-MoO3 sol dipping. Subsequently, TiC0.7N0.3@WC-MoC2 core-shell structural microspheres were successfully obtained by carburizing the precursor at 900 °C in a flowing mixture of CH4 (20 ml·min-1) and H2 (200 ml·min-1) for 2 h. Then TiC0.7N0.3@WC-MoC2-15Co cermets were prepared utilizing the core-shell powders by spark plasma sintering (SPS). Powders of the precursors with TiC0.7N0.3@WO3-MO3 microspheres, TiC0.7N0.3@WC-MoC2 microspheres and TiC0.7N0.3@WC-MoC2-15Co cermets were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray diffraction (XRD). The obtained TiC0.7N0.3@WC-MoC2 microspheres have a dense WC-MoC2 coatings shell. The thickness of the shell could be easily controlled by adjusting the number of sol dipping cycles. It was found that the TiC0.7N0.3@WC-MoC2 microspheres were more beneficial to fabricate the "core-rim" structures by SPS.     

Controllable preparation and superior rate performance of spinel LiMn<Subscript>2</Subscript>O<Subscript>4</Subscript> hollow microspheres as cathode material for lithium-ion batteries

Spinel LiMn₂O₄ microspheres and hollow microspheres with adjustable wall thickness have been prepared using controllable oxidation of MnCO₃ microspheres precursors and following solid reactions with lithium salts. Scanning electron microscopy (SEM) investigations demonstrate that the microsphere morphology and hollow structure of precursors are inherited. The effect of hollow structure properties of as-prepared LiMn₂O₄ on their performance as cathode materials for lithium-ion batteries has been studied. Electrochemical performance tests show that LiMn₂O₄ hollow microspheres with small wall thickness exhibit both superior rate capability and better cycle performance than LiMn₂O₄ solid microspheres and LiMn₂O₄ hollow microspheres with thick wall. The LiMn₂O₄ hollow microspheres with thin wall have discharge capacity of 132.7 mA·h·g^-1 at C/10 (14.8 mA·g^-1) in the first cycle, 94.1% capacity retention at C/10 after 40 cycles and discharge capacity of 116.5 mAh·g^-1 at a high rate of 5C. The apparent lithium-ion diffusion coefficient (D _app) of as-prepared LiMn₂O₄ determined by capacity intermittent titration technique (CITT) varies from 10^-11 to 10^-8.5 cm²·s^-1 showing a regular “W” shape curve plotted with test voltages. The Dapp of LiMn₂O₄ hollow microspheres with thin wall has the largest value among all the prepared samples. Both the superior rate capability and cycle stability of LiMn₂O₄ hollow microspheres with thin wall can be ascribed to the facile ion diffusion in the hollow structures and the robust of hollow structures during repeated cycling.     

Preparation of Ni/PZT core-shell nanoparticles and their electromagnetic properties

The Ni nanoparticles coated with Pb(Zr,Ti)O_3(PZT) were synthesized by a sol-gel method and in situ reaction. And their structure, oxidation resistance, and electromagnetic properties were investigated. The X-ray diffraction patterns(XRD) exhibited that a small amount of impure phase characterized to Ni(OH)_2 was detected from the ammonia-treated Ni nanoparticles and the ammonia-treated Ni nanoparticles coated with PZT. After being pre-treated with aqueous ammonia, the PZT coating layer was more uniform and about 10 nm in thickness. The oxidation resistance of the ammonia-treated Ni nanoparticles coated with PZT, compared with that of the non-treated ones, was improved by about 66 ℃. The PZT shell layer prepared by in-situ reaction can greatly reduce the dielectric constant and improve the natural resonance loss at high frequency, so as to obtain the optimal impedance matching performance of the electromagnetic wave transmission.     

Phase Evolution and Oxidation Resistance of YSZ/(Ni,Al) Composite Coatings in CH<Subscript>4</Subscript> Atmosphere

YSZ/(Ni, Al) composite coatings with different Ni:Al mole ratios were deposited on superalloy Inconel 600 by electrophoretic deposition (EPD) technique, followed by sintering in CH₄ atmosphere at 1 100 °C for 2 h and isothermally oxidation at 1000 °C for 50 h. After sintering at 1100 °C for 2 h in CH₄ atmosphere, besides ZrC and t-ZrO₂ phases, the phase constitutes of Ni:Al mole ratios with 1:3, 1:2, and 1:1 were (Zr, Al)C, AlNi₃ and Ni phases, respectively. A remarkable difference in the oxidation behaviors of YSZ/(Ni, Al) composite coatings with different Ni:Al mole ratios was observed. For YSZ(Ni:Al=1:3) coated sample, oxidation at 1000 °C causes decomposition of the (Zr,Al)C solid solution to metallic Al, and then most of the Al is oxidized to Al₂O₃. For the YSZ(Ni:Al=1:2) coated sample, oxidation at 1000 °C mainly causes decomposition of the AlNi₃ phase. For YSZ(Ni:Al=1:1) coated sample, after oxidation at 1000 °C, most of the Ni is oxidized to NiO phase, and tolerated 50 h of oxidation and finally cracked and spalled from the specimen. YSZ(Ni:Al=1:3) and YSZ(Ni:Al=1:2) coated samples show superior oxidation resistance than that of YSZ coating. The different oxidation resistance mechanisms of YSZ/(Ni, Al) composite coatings sintered in CH₄ atmosphere were discussed.     

Synthesis of γ-Al2O3 nanoparticles by chemical precipitation method

Highly pure active γ-Al₂O₃ nanoparticles were synthesized from aluminum nitrate and ammonium carbonate with a little surfactant by chemical precipitation method. The factors affecting the synthesis process were studied. The properties of γ-Al₂O₃ nanoparticles were characterized by DTA, XRD, BET, TEM, laser granularity analysis and impurity content analysis. The results show that the amorphous precursor Al(OH)₃ sols are produced by using 0.1 mol/L Al(NO₃)₃ · 9H₂O and 0.16 mol/L (NH₄)₂CO₃ · H₂O reaction solutions, according to the volume ratio 1.33, adding 0.024% (volume fraction) surfactant PEG600, and reacting at 40 °C, 1 000 r/min stirring rate for 15 min. Then, after stabilizing for 24 h, the precursors were extracted and filtrated by vacuum, washed thoroughly with deionized water and dehydrated ethanol, dried in vacuum at 80°C for 8 h, final calcined at 800 °C for 1 h in the air, and high purity active γ-Al₂O₃ nanoparticles can be prepared with cubic in crystal system, O _H ⁷ -FD3M in space group, about 9 nm in crystal grain size, about 20 nm in particle size and uniform size distribution, 131. 35 m²/g in BET specific surface area, 7 – 11 nm in pore diameter, and not lower than 99.93% in purity. Foundation item: Project(03JJY3015) supported by the Natural Science Foundation of Hunan Province     

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.     

Co2O3-doping effect on the formation of 3CaO·3Al2O3·CaSO4

The Co₂O₃-doping effect on the formation of 3CaO·3Al₂O₃·CaSO₄ from CaCO₃-Al₂O₃-CaSO₄·2H₂O mixtures was investigated by means of SO₂ emission behavior, chemical analysis, X-ray diffraction, differential thermal analysis and scanning electron microscopy. The experimental results show that Co₂O₃ addition increases the reactivity of the CaCO₃-Al₂O₃-CaSO₄·2H₂O system significantly, by reducing SO₂ emissions in combustion and f-CaO contents in the clinkers, promoting the nucleation and growth of 3CaO· 3Al₂O₃·CaSO₄, and intensifying the formation of 3CaO·3Al₂O₃·CaSO₄. Moreover, Co₂O₃ addition lowers the formation temperature of 3CaO·3Al₂O3·CaSO₄ by 18 °C, and similarly increases the thermal stability of it at a wider temperature range.     

Effect of CaCO3 on hydration characteristics of C3A

Hydration products and morphology characteristics of C₃A (tricalcium aluminate)-CaCO₃-H₂O system were studied by means of XRD, DSC, FTIR spectrum analysis and SEM. The results indicate that, the new phases, i.e., C₃A·0.5CaCO₃·0.5Ca(OH)₂·11.5H₂O and C₃A·CaCO₃·11H₂O are found in this system due to the activity of CaCO₃; the formation of C₄AH₁₃ and C₂AH₈ is prohibited and the generation of C₃AH₆ is delayed in the early hydration process. C₃A·0.5CaCO₃·0.5Ca(OH)₂·11.5H₂O is not stable and will be totally transferred within 24 h; C₃A·CaCO₃·11H₂O exists stably once formation, and its flake-like crystalline phases in the early hydration transform to long rod shape, and to finally fine-needle at 28 d.     

Preparation of microsized single-crystalline Co_3O_4 by high-temperature hydrolysis

Microsized single-crystalline Co3O4 has been synthesized by high-temperature hydrolysis of CoCl2·2H2O at 600 °C.The samples were characterized by powder X-ray diffraction(XRD),scanning electron microscopy(SEM) and transmission electron microscopy(TEM).The results reveal that the as-prepared powders are microsized single-crystalline Co3O4 with cubic spinel structure.An increase in the high-temperature hydrolysis time results in the evolution of particle shapes from cube to quasi-sphere,and then to octahedron...     

Formation of CuS pineal microspheres via a pyridine-solvothermal process

CuS pineal microspheres congregated from interleaving nanoflakes with thickness of 40 to 200 nm were synthesized by a pyridine-solvothermal process via the reaction between cupric chloride(CuCl2·2H2O) and thioacetamide(TAA,CH3CSNH2).The products were characterized by X-ray diffraction and scanning electron microscopy.UV-Vis absorption spectrum,excitation and photoluminescence spectra of CuS pineal microspheres were obtained at room temperature to investigate their optical properties.A possible growth mechanism on the formation of CuS pineal microspheres is proposed.The factors influencing the evolution of morphologies of CuS crystals including the dosage of the reactants,surfactant,and sulphur-source were also analyzed.     

Synthesis and characterization of arsenate antimonic acid AAAc(1 : 1)

The AAAc(1 : 1) was synthesized in water by As₂O₃ and Sb₂O₃ with molar ratio of 1 : 1. AAAc(1 : 1) was characterized by Raman, IR, TG/DTG, DSC, XPS and XRD. The results show that there are four peaks to v _s of As-OH, As-O-Sb, Sb-OH and Sb-O-Sb in Raman spectra of AAAc(1 : 1) at 100 – 1 000 cm⁻¹. The solution of AAAc(1 : 1) was also titrated with KOH solution. The titration results show that AAAc(1 : 1) is a hexabasic acid with dissociation constants of k ₁=3.62 × 10⁻², k ₂=3.05 × 10⁻³, k ₃=6.43 × 10⁻⁶, k ₄ =9.78 × 10⁻⁸, k ₅=1.32 × 10⁻¹¹, k ₆=3.87 × 10⁻¹². AAAc(1 : 1) has a good solubility and stability in water, its solid obtained by free volatilizing water from its solution under air at ambient temperature is amorphous. Chemical and thermal analysis show that the composition of AAAc(1 : 1) is As₂O₅ · Sb₂O₅ · 8H₂O in air at 25 °C. AAAc(1 : 1) has the structure of AsO(OH)₂-OH-Sb(OH)₄-O-Sb(OH)₄-OH-AsO(OH)₂ or As(OH)₃-O-Sb(OH)₄-O-Sb(OH)₄-O-As(OH)₃ (isomerism) through experimental determination and geometry optimization. Foundation item: Project(50274075) supported by the National Natural Science Foundation of China     

Modification of LiCo1/3Ni1/3Mn1/3O2 cathode material by CeO2-coating

LiCo_1/3Ni_1/3Mn_1/3O₂ was coated by a layer of 1.0 wt% CeO₂ via sol-gel method. The bared and coated LiMn_1/3Co_1/3Ni_1/3O₂ was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), cyclic voltammogram (CV) and galvanotactic charge-discharge test. The results show that the coating layer has no effect on the crystal structure, only coating on the surface; the 1.0 wt% CeO₂-coated LiCo_1/3Ni_1/3Mn_1/3O₂ exhibits better discharge capacity and cycling performance than the bared LiCo_1/3Ni_1/3Mn_1/3O₂. The discharge capacity of 1.0 wt% CeO₂-coated cathode is 182.5 mAh·g⁻¹ at a current density of 20 mA·g⁻¹, in contrast to 165.8 mAh·g⁻¹of the bared sample. The discharge capacity retention of 1.0 wt% CeO₂-coated sample after 12 cycles reaches 93.2%, in comparison with 86.6% of the bared sample. CV results show that the CeO₂ coating could suppress phase transitions and prevent the surface of cathode material from direct contact with the electrolyte, thus enhance the electrochemical performance of the coated material.     

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     

Modification of natural graphite using pitch through dynamical melt-carbonization

The graphite was modified using pitch through dynamical melt-carbonization, and the effects of modification temperature and the amount of pitch on the characteristics of graphite were investigated. The structure and characteristics of the graphite were determined by X-ray diffractometry(XRD), scanning electron microscopy(SEM), particle size analysis and electrochemical measurements. The results show that the modified graphite has a disordered carbon/graphite composite structure, larger average particle diameter, greater tap density, and better electrochemical characteristics than the untreated graphite. The sample coated with 10% pitch dynamical melt-carbonized at 400 ℃ for 3 h and heat-treated at 850 ℃ for 2 h has better electrochemical performances with a reversible capacity of 360.5 mA·h/g, a irreversible capacity of 41.0 mA·h/g, and an initial coulombic efficiency of 89.8% compared with natural graphite and disordered carbon. The cycling stability of the Li/C cell with modified graphite as anodes is improved, and its capacity retention ratio at the 30th cycle is up to 94.37%.     

Supporting of nickel(II) acenaphthenediimine with free amino group for ethylene polymerization

Bis (4-(4-amino-3, 5-diethylbenzyl)-2, 6-diethylphenylimino) acenaphthene] dichloronickel (NiLCl₂) was prepared and supported on SiO₂ modified by methyl trichlorsilane(S-1) and on SiO₂-MgCl₂/TiCl₄ (S-2) respectively. Two supported catalysts S-1 and S-2 used as catalysts for ethylene polymerization were studied and the influences of various polymerization conditions, including the polymerization temperature, cocatalysts, Al/Ni molar ratio on the catalytic activity, branching degree and branch length of PE were also investigated. The experimental results show that the supported catalysts exhibit higher catalytic activity for ethylene polymerization, the highest catalytic activity of S-1 using AlEt₂Cl as cocatalyst at 50°C, reaching 5.8×10⁵gPE/molNi··h, and needed lower Al/Ni molar ratio compared to homogeneous analogue.     

Preparation of ITO nano-powders by hydrothermal-calcining process

1 INTRODUCTIONSn-doped In2O3(ITO) is one kind of n-typesemiconductor material[1].It has excellent electro-optical properties , such as electrical conductivityand high transparency under visible light[2],andiswidely used in electronic , transparent electrode ,solar cells and electro-irradiance , especially inscreen display[3 ,4].Recently nearly half of the met-al indium has been used to prepare ITO materialsin the developed countries[5], such as Japan, A-merica ,France and so on.So the…