5Mg(OH)2·MgSO4·2H2O晶须生长过程中的形貌研究

Using MgSO₄ and NaOH solutions as starting materials, the whisker of 5Mg(OH)₂·MgSO₄·2H₂O has been prepared by hydrothermal method at 160℃ for different time. The whisker was separated, washed by water, ethanol and ether,and characterized by chemical analysis, XRD, IR and microphotography. The growth time of whisker would affect its morphology.     

三元体系Cu(NO3)2-EBU-H2O 30℃时等温溶度及其新相研究

The isothermal solubility of the ternary system Cu(NO₃)₂-EBU-H₂O at 30℃ has been studied for the first time and the solubility diagram and refractive indices diagram have been given. New phase Cu(NO₃)₂·2EBU has been found in this system， which dissolves incongruently in water .The phase has been characterized by element anal-ysis， IR spectra and X-ray diffraction powder analysis.     

MgSO4·5Mg(OH)2·3H2O的水热合成及反应时间对其形貌的影响

Both whisker and nanometer MgSO₄·5Mg(OH)₂·3H₂O(MOS) were prepared by hydrothermal method at 140℃ for different times， using NaOH and MgSO₄·7H₂O as raw materials. The MgSO₄·5Mg(OH)₂·3H₂O part- icles were characterized by powder X-ray diffraction(XRD)，thermal analysis(TGA-DSC)， infrared spectroscopy(FT-IR)，transmission electron microscopy(SEM) and scanning electron microscopy(TEM). The size distribution in whisker-like and nanocrystalline materials are in the range of 10～50μm and 10～20nm respectively. The whisker MOS is metastable phase in MgSO₄-NaOH-H₂O system at 140℃，whereas nanometer MOS is stable phase.     

Cs2SO4-C2H5OH-H2O三元体系30℃和50℃的平衡溶解度研究

The solubilities of Cs₂SO₄-C₂H₅OH-H₂O ternary system at 30℃ and 50℃ have been studied using microe-quipment for solubility determination. There appears two phases, alcoholic phase, water phase in the liquid phase. The solubilities of Cs₂SO₄ in water, C₂H₅OH and mixed solvent have been determined. The phase diagram indicated that C₂H₅OH might be salted out by Cs₂SO₄ from this system and the equilibrium solid phase is Cs₂SO₄.     

非晶态羧酸盐法合成NTC热敏陶瓷用Ni1.0Co0.2Mn1.8O4纳米粉体的研究

Nano-crystalline Ni_1.0Co_0.2Mn_1.8O₄ powders were synthesized via non-crystalloid precursor method. The results on the precursor by XRD and IR techniques show that the stable non-crystalloid precursor could be formed by adding oleic acide and adjusting the pH values. The dried precursor exhibited auto-catalytic combustion behavior. After being calcined at 800 ℃, the Ni_1.0Co_0.2Mn_1.8O₄ powders with spinel structure were obtained. It has been demonstrated that the synthesized powder is well dispersed and with higher sintering activity. The Model of non-crystalloid precursor has been suggested. The reaction mechanism has also been proposed.     

电镀烧结法制备Ti/SnO2-Sb2O4电极的研究

The Ti/SnO₂-Sb₂O₄ electrode has been prepared by the electroplate-sinter method. The effect of SbCl₃ adding amount and sintering temperature on its electrode lifetime and oxygen evolution potential were investigated by means of EDX, SEM and XRD analysis. The results indicated that the electrode appeared the best performance when the SbCl₃ adding amounts was 0.2g and the sintering temperature was 550℃. In optimized conditions Ti substrate was entirely covered by SnO₂-Sb₂O₄ and the combinations among them were tight. Due to the use of electroplate method, the electrical conductivity, the oxygen evolution potential and the electrode lifetime were increased, so the elec-tro-catalytic activity and the electrochemical stability of the prepared electrode were found to be superior.     

掺镍型层状LixNiyMn1-yO2正极材料的合成与电性能研究

A kind of cathode material of layered Li_xNi_yMn_1-yO₂ characterized with the O2 type has been synthesized by a simple method. Its precursor Na_xNi_yMn_1-yO₂ has been prepared from manganese dioxide， nickel hydroxide and sodium carbonate at high temperature in air and quickly cooled in cold water， then it has been exchanged by the melted LiNO₃ at 300～400℃ in air. The effects of calcine-temperature for the precursors and its compositions (the content of Na and Ni) on the electrochemical properties of the material Li_xNi_yMn_1-yO₂ have been investingated by XRD and electrochemical tests. The results show that the sample Li_0.7Ni_0.3Mn_0.7O₂， has the best electrochemical properties which shows only one charge-discharge potential stage of 2.8～3.0V and has a high specific capacity over 180mAh·g^-1 cycled between 2.0～4.20V. A significant structure transformation to the spinal-type phase has not been found in the charge-discharge cycling and the discharge specific capacity around 165mAh·g^-1 has re-mained after the 20th cyclings for the material.     

硬脂酸法制备超细K2La2Ti3O10及其酸交换性质研究

A new stearic acid method(SAM) has been used to prepare ultrafine K₂La₂Ti₃O₁₀ nanocrystalline. Each state of synthesis process was followed by the use of FT-IR analysis. The resulting materials have been characterized by means of XRD， TEM， BET surface area analysis. The acid-exchanging property of the obtained product was also studied. The experimental results showed that comparing with the product of traditional solid-state reaction， the particle size of the K₂La₂Ti₃O₁₀ synthesized by SAM is greatly reduced， BET surface area is high(more than 11.83m²·g^-1) and has different acid-exchanging properties. It can be easily exfoliated in 2mol·L^-1 HNO₃ so-lution.     

通过β-FeOOH纳米棒无序聚集制备α-Fe2O3中空球

The α-Fe₂O₃ hollow spheres have been synthesized through the random aggregation of β-FeOOH nanorods in the C₂H₅OH/H₂O system. The phase transformation and the morphologies of the α-Fe₂O₃ hollow structure were investigated with XRD， SEM， TEM and selected area electron diffraction (SAED). These studies indicate that the second step is a dissolution-recrystallization process. Furthermore， the formation mechanism of the hollow spheres has been discussed. It is found that the presence of H₂O in the reaction system is essential to the final formation of the hollow spheres.     

Li2CO3、NiO和电解MnO2合成高容量LiNi0.5Mn1.5O4及其表征

Well-developed crystalline LiNi_0.5Mn_1.5O₄ was prepared by solid-state reaction using Li₂CO₃, NiO and electrolytic MnO₂ at high heating and cooling rate. X-ray diffraction (XRD) patterns and scanning electron microscopic (SEM) images showed that LiNi_0.5Mn_1.5O₄ synthesized at 900 ℃ and 950 ℃ had cubic spinel structure with clearly defined shape. LiNi_0.5Mn_1.5O₄ spinel phase decomposed at 1 000 ℃ accompanying with structural and morphological degradation. TG measurement revealed that the weight loss during heating process could be mostly gained in cooling process, and the upward tendency of weight loss during heating process decreased, while that of irreversible weight loss rapidly increased with the increase of temperature. LiNi_0.5Mn_1.5O₄ powders prepared at 900 ℃ for 12 h delivered the maximum discharge capacity of 134 mAh·g^-1 with good cyclic performance at 2/7 C. In addition, by adjusting the calcination time at 900 ℃, the capacity and cycling performance of LiNi_0.5Mn_1.5O₄ were further enhanced.     

[Zn(en)3]SO4配合物大尺寸单晶的水热法生长和表征

Large size single crystals of [Zn(en)₃]SO₄ have been successfully grown by a hydrothermal process at 160℃ for 24h， using CuSO₄·5H₂O， ethylene diamine and reductive Zn powder as reactants. The diameters of the single crystals are range from 0.5mm to 1mm， and lengths reach up to 20mm. The single crystals were characterized by XRD analysis， FTIR and UV-Vis spectrum absorption measurements. The single crystal was confirmed to be [Zn(en)₃]SO₄ by performing powder diffraction of the single crystal. X-ray diffraction of the single crystals shows (100)-face to be cleavage face. The diffraction peaks are sharp and rocking curve for 200 diffraction has a narrow FWHM (the full width at half maximum)， which indicate the single crystal of [Zn(en)₃]SO₄ is perfect with less lattice distortion and defects. The single crystal appears transparent，and has constant weak absorption in UV-Vis spectrum region，which could be used as a novel optical crystal material.     

中温固体氧化物燃料电池复合阴极La1.6Sr0.4NiO4-Ce0.9Gd0.1O1.9的制备及性能研究

Composite cathodes consisting of -La_1.6Sr_0.4NiO₄(LSN) and -Ce_0.9Gd_0.1O_1.9(CGO) has been prepared for intermediate temperature solid oxide fuel cell (IT-SOFC). The chemical stability, microstructures and electrochemical performance of the cathode have been investigated using XRD, SEM and AC impedance spectroscopy. Results showed that strong bonding was formed between the composite electrodes and CGO electrolytes after the electrodes were fired at 1 050 ℃ for 4 hours. The polarization resistance changed with oxygen partial pressure, suggesting that charge transfer process was the rate limiting step for electrochemical oxygen reduction at the composite cathodes. Area specific resistance (ASR) for a LSN-40CGO composite cathode was 0.76 Ω·cm² at 700 ℃, which was four times lower than that of a pure LSN cathode. 1.7％ decrease of the cathode current density was observed in the stability test of the composite cathode.     

Yb(Cl4)3·3H2O-18C6-C2H5OH体系(25℃)的相化学研究及固态配合物的合成与性质

The solubilities of Yb(ClO₄)₃·3H₂O-18C6-C₂H₅OH ternary system at 25 were invstigated by a semimicro method for study of phase equilibrium.and the refractive indexes of saturated solutions were determined.The behavior of water in this system during the equilibrium was examined.The results indicate that there are two kinds of complexes formed in the system, their chemical compositions are: Yb(ClO₄)₃·18C6·3H₂O·2C₂H₅OH (I) and Yb(ClO₄)₃ 18C6·3H₂O·C₂H₅OH.Both are incongruently soluble in EtOH.The influences of rare earth ions and salt anions on formation of complexes were discussed.The two solid complexes have been prepared, and their composihons and properties have been investigated by chemical analysis, IR, DTG and DSC.According to the DSC, the enthalpies of some steps during the decomposition have been obtained for complexes (Ⅲ)and (Ⅳ).     

CeOHCO3和CeO2束状纳米结构的制备及表征

The cantaloupe-like particles of CeOHCO₃ were synthesized in aqueous solution by using cetyltrimethylammonium bromide (CTAB) as soft template. Then, the bunchiness rods of CeO₂ were obtained by calcining CeOHCO₃ at 450 ℃. The results of thermogravimetric/differential thermal analysis reveal that an endothermic reaction with decomposition is involved in the transformation process from CeOHCO₃ to CeO₂. By scanning electron microscopy and X-ray diffraction analysis, it is found that the orthorhombic phase CeOHCO₃ particles are constituted of short nanorods with diameters ranging from several tens nm to over 100 nm, and the cubic phase CeO₂ rods are composed of small particles with diameter ca. 15 nm. From the results of UV-Vis absorption and photoluminescence analysis, it is found that the CeO₂ possess abundant defects, and the band gaps of the CeO₂ and CeOHCO₃ are ca. 2.70 eV and 3.87 eV, respectively.     

发光材料BaAl2Si2O8∶Eu2+的物相结构与发光性能

A phosphor, Ba_0.97Al₂Si₂O₈∶Eu²⁺, was synthesized by high temperature solid-phase method at different temperatures. The samples were characterized by TG/DTA, XRD and fluorescence spectroscopy. The results show that the main phase for host of these luminescence materials is barium feldspar BaAl₂Si₂O₈∶Eu²⁺ and there is a transition from hexagonal crystal system to monoclinic crystal system in the process of the sintering of barium feldspar. The luminescent phenomen of barium feldspar with hexagonal structure can not be observed under the excitation of ultraviolet lamp of 365 nm while the barium feldspar with monoclinic structure has excellent luminescence properties. The excitation spectra of all these samples show broad band spectra ranging from 250～390 nm with peak at λ_ex of 357 nm,which indicates that these samples can be effectively excited by near ultraviolet ; the emission spectra range from 380～600 nm with peak at λ_em of 433 nm. The luminescent intensity increases then decreases with the concentration of doping Eu²⁺ ions. When the concentration of dopants is 2.5mol%, the luminescent intensity reaches the maximum value. When the concentration of Eu²⁺ ions changes from 0.5mol% to 2.5mol%, the emission peak has a red shift from 427 nm to 440 nm.     

Si5P6O25∶Tb3+的结构与荧光性质

Tb³⁺ ions were incorporated in P-Si matrix material through a sol-gel process. Luminescence properties of Tb³⁺ as a function of dopant， firing temperature， composition and structure of matrices were investigated. The gels synthesized by the reaction of P₂O₅ or H₃PO₄ with tetraethoxy silane and TbCl₃ as dopant were fired in air from the temperature 25～1000℃ to form P-Si crystalline phase. The crystal structure was determined by powder X-ray diffraction. Si₅O(PO₄)₆ were the only crystalline phase and belong to hexagonal crystal system. The emission of ⁵D₄-⁷F₅(～545nm) transition of Tb³⁺ in the P-Si system is composed of two peaks. The amount of doping Tb³⁺ varied from 0.664% to 1.644%， and no obvious concentration quenching was observed in this doping concentra-tion range. The intensity of Tb³⁺ emission increased with firing temperature increasing and becomes stable at 800～1000℃.     

LiAlO2细粉料的制备及反应机理研究

As a functional inorganic material, LiAlO₂ was focused on widely, especially in the field of tritium breeder of fusion reactor. In this article, the proper reaction conditions and mechanism to synthesis the γ-LiAlO₂ by solid state method are considered. In the experiments, it has been found that the phase of β- and γ-LiAlO₂ are only produced by the reaction of LiOH and Al₂O₃, while the α- and γ-LiAlO₂ can be obtained by the reaction of Li₂CO₃ and Al₂O₃. As compared with Li₂CO₃ and Al₂O₃ reacted at 900～1000℃ for the preparation of γ-LiAlO₂, the γ-LiAlO₂ can also be made by the reaction of LiOH and Al₂O₃ at some more lower temperatures that is due to the bulk diffuse mech-anism. But the former can get better crystal and have smaller particles for the mechanism of surface fast reaction. As a result, the sub-micron γ-LiAlO₂ powders with the diameter less than 0.3μm are obtained.     

高分子网络法制备纳米NiO超细粉的研究

Superfine NiO powders，15～50nm ca.， with single phase and uniform particle size have been prepared from Ni(NO₃)₂ by a polymer-network gel process. The results demonstrate that the distribution of the particle sizes of final oxides depends on the heated temperature，time and concentration of original nickel nitrate solution. The control of particle size of nano-NiO powders can be realized by the control of the condition of the process.     

准球形α-Fe2O3的形成过程研究

The formation process of pseudo-spherical α-Fe₂O₃ particles obtained through the hydrolysis of 0.01 mol·L^-1 FeCl₃ solution was studied by means of TEM and XRD. The results show that the growth of α-Fe₂O₃ nuclies is through the diffusion mechanism. Although the presence of CTAB in the FeCl₃ solution has no effect on the growth process of pseudo-spheric α-Fe₂O₃ particles, more uniform particles are obtained, and the particles are self-assembled to form two-dimensional ordered structure due to the effect of CTAB. The optical character of these α-Fe₂O₃ particles was investigated, and the band-gap of which is about 2.49 eV.     

半化学法制备PMW-PNN-PT粉体的反应机理研究

The mechanism of perovskite 0.1Pb(Mg_1/2W_1/2)O₃-0.6Pb(Ni_1/3Nb_2/3)O₃-0.3PbTiO₃ (abbreviated PMW-PNN-PT) phase formation by Semichemical Method has been studied. The precursors were prepared by adding aqueous solution of Mg(Ac)₂ and Ni(AC)₂ rather than solid MgO and NiO to the alcoholic slurry of PbO, WO₃, Nb₂O₅ and TiO₂. The TG-DTG and DSC of the precursors and XRD analysis of the powders at various calcination temperature showed that the mechanism of this method was different from that of the conventional mixed oxide method. The aqueous Mg(Ac)₂ and Ni(Ac)₂ reacted with PbO to form basic lead acetate, basic magnesium acetate and basic nickel acetate and so on. With the increase of calcination temperature these basic salt decomposed to form nascent PbO, MgO and NiO, which improved the reactivity and distribution of PbO, MgO and NiO. In addition, the formation of PbWO₄ and pyrochlore phase Pb₃Nb₂O₈ in the process was in favor of the pervoskite PMW-PNN-PT phase formation. At the calcining temperature of 850 ℃, the perovskite phase reached 98%.