含钛磷酸盐玻璃NaTi2(PO4)3-0.9Ca3(PO4)2的析晶行为

利用差热分析、X射线衍射仪、液氮吸附BET孔经测试仪对组成为NaTi2(PO4)3-0.9 Ca3(PO4)2的含钛磷酸盐玻璃的析晶行为进行了研究.通过对该玻璃相继进行成核、析晶和酸浸泡处理制备了NaTi2(PO4)3骨架多孔微晶玻璃.证明该玻璃在646℃8h成核处理过程中产生了旋节分解特征的成分偏聚,形成了富TiO2玻璃相和富CaO玻璃相交错生长的连通结构,成核处理后的玻璃在738℃析晶过程中依次在富钛相和富钙相中析出NaTi2(PO4)3和β-Ca3(PO4)2.成核过程对析晶的促进作用是通过促进NaTi2(PO4)3的析出而实现的.     

Crystal structure of uranyl μ3-oxoacetate [(UO2)3(μ3-O)2(OOCCH3)2(H2O)2]

The crystal structure of [(UO₂)₃(₃-O)₂(OOCCH₃)₂(H₂O)₂] consists of uranium coordination polyhedra (CPs) combined via common equatorial edges into ribbons, with ₃-O atoms being common for three CPs. The structure was compared with that of known complexes with ₃-oxo atoms.Translated from Radiokhimiya, Vol. 46, No. 5, 2004, pp. 396–400.Original Russian Text Copyright © 2004 by Charushnikova, Krot, Starikova.     

Multifunctional γ-Fe2O3@Ca3(PO4)2@YPO4:Tb,Ce nanocomposites as a potential drug carrier

Multifunctional γ-Fe₂O₃@Ca₃(PO₄)₂@YPO₄:Tb³⁺,Ce³⁺ nanocomposites were synthesized using an easy direct-precipitation method. The nanocomposites had a monodispersed spherical morphology with a narrow size distribution, and dispersed well in water. The nanocomposites showed the characteristic emission peaks of Ce³⁺ (5d–4f) and Tb³⁺ (⁵D₄–⁷F₃ to ⁵D₄–⁷F₆). Magnetism measurements revealed that the samples were nearly superparamagnetic. The multifunctional nanocomposites were used for in vitro drug delivery tests under ambient conditions, and we discuss the influence of different media on the release of cisplatin (cis-diamminedichloroplatinum). We assessed the loading and release performance for cisplatin by means of UV–visible spectrophotometry. Our findings will provide guidance for engineering similar multifunctional nanocomposites for use in future drug delivery applications.     

Room temperature metathetic synthesis and characterization of α-hopeite, Zn3(PO4)2·4H2O

The synthesis of crystalline zinc phosphates (α-hopeite phase) through the metathetic pathway has been investigated. The reaction has been carried out by room-temperature grinding. High lattice energy of the by-product NaCl has driven the reaction in the forward direction, and as a result, stable phosphate phases have been synthesized. Reaction of a different phosphorus source (like Na₃PO₄, Na₂HPO₄, NaH₂PO₄, and K₂HPO₄) with ZnCl₂ has been attempted. The structural, vibrational, thermal, optical, and chemical properties of synthesized powders are determined by powder X-ray diffraction (XRD), scanning electron microscope (SEM), thermogravimetric analysis (TGA), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FTIR) and diffused reflectance spectra (DR) in the UV-vis range. The direct band gap of the title compound was determined to be 3.6 ± 0.2 eV.     

Synthesis and properties of β-Ga2O3 nanostructures

A novel method was utilized to synthesize one-dimensional β-Ga₂O₃ nanostructures. In this method, β-Ga₂O₃ nanostructures have been successfully synthesized on Si(111) substrates through annealing sputtered Ga₂O₃/Mo films under flowing ammonia in a quartz tube. The as-obtained samples were analyzed in detail using the methods of X-ray diffraction (XRD), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM) and energy dispersive X-ray spectroscopy (EDX) attached to the HRTEM instrument. The results show that the formed nanostructures are single-crystalline Ga₂O₃. The annealing temperature has an evident influence on the morphology of the β-Ga₂O₃ nanostructures. The growth mechanism of the β-Ga₂O₃ nanostructures is also discussed by conventional vapor-solid (VS) mechanism.     

Magnetic, electrical, and optical properties of (HgS)1.5(Al2S3)0.5?Mn? and (HgS)1.5(In2S3)0.5?Mn? crystals

We have studied the magnetic, electrical, and optical properties of (HgS)_1.5(Al₂S₃)_0.5〈Mn〉 and (HgS)_1.5(In₂S₃)_0.5〈Mn〉 crystals and determined their magnetic and band structure parameters. The magnetic (Faraday method) and transport (four-probe method) properties of the (HgS)_1.5(Al₂S₃)_0.5〈Mn〉 and (HgS)_1.5(In₂S₃)_0.5〈Mn〉 crystals were investigated in the ranges T = 77−300 K and H = 20−320 kA/m. The magnetic susceptibility data suggest that the magnetic properties of the crystals can be understood in terms of Mn-S-Mn-S clusters. The Hall coefficient of the crystals is temperature-independent. The electrical conductivity of (HgS)_1.5(Al₂S₃)_0.5〈Mn〉 varies little with temperature and has a maximum, and that of (HgS)_1.5(In₂S₃)0.5〈Mn〉 shows metallic behavior and is a nearly linear function of temperature. The thermopower of the crystals increases with temperature. Optical data attest to direct allowed interband optical transitions. The magnetic and band structure parameters of the crystals are determined.     

Synthesis and electrochemical performance of β-Co(OH)2

A novel electro-active material was synthesized by precipitation under high levels of supersaturation. The compound was pure β-Co(OH)₂ with hexagonal crystal structure by XRD analysis, and it was flake-shaped, 50–200 nm in particle size and ∼20 nm in thickness by FE-SEM observation. The quasireversible electrochemical reaction between β-Co(OH)₂ and Co upon charging/discharging produced a maximum discharge capacity of 462 mAh g⁻¹, and furthermore the discharge capacity retained 97.6% of the initial capacity at the 100th cycle. These findings highlight the potential for β-Co(OH)₂ compound in applications to negative electrode materials of alkaline rechargeable batteries.     

Reducing ultra-low thermal expansion of β-Zr2O(PO4)2 by substitutions?

The ultra-low thermal expansion of β-Zr₂O(PO₄)₂ could still be reduced by chemical modifications, according to previous works on uranium and thorium IV homologues that evidenced a contracting effect of big cations. However, the present study shows that the only isovalent cations likely to substitute for Zr^IV or P^V are either harmful, or unstable, chemically or thermally. Furthermore, aliovalent modifications seem to be forbidden by the crystal structure of the material, leaving probably very few perspectives of improvement. Vanadium however improves significantly the crystallinity of the material and lowers the α-β transition temperature.     

Synthesis of ZnGa2O4 nanowires with β-Ga2O3 templates and its photoluminescence performance

This paper focuses on a new but much simple approach in synthesizing cubic spinel-structure ZnGa₂O₄ nanowires through the reaction of β-Ga₂O₃ nanowires templates and ZnO vapor at high temperature. Characterization has been achieved by means of X-ray diffraction, scanning electron microscopy and transmission electron microscopy. The length of as-synthesized ZnGa₂O₄ nanowires is scaled over 10 μm and the diameter is 80 nm respectively. It has been noticed that the concentration of ZnO vapor plays an important role for synthesizing ZnGa₂O₄ nanowires. And with different concentration of ZnO vapor, the very nanowires could be compounded in the form of β-Ga₂O₃:ZnGa₂O₄, ZnGa₂O₄ and ZnO:ZnGa₂O₄. The corresponding photoluminescence emission bands centered at 460 nm, 405 nm and 381 nm have also been observed.     

Preparation, characterization and conductivity studies of Li3?2xAl2?xSbx(PO4)3

New NASICON type materials of composition, Li_3−2x Al_2−x Sb _x (PO₄)₃ (x = 0·6 to 1·4), have been prepared and characterized by powder XRD and IR. D.C. conductivities were measured in the temperature range 300–573 K by a two-probe method. Impedance studies were carried out in the frequency region 10²−10⁶ Hz as a function of temperature (300–573 K). An Arrhenius behaviour is observed for all compositions by d.c. conductivity and the Cole-Cole plots obtained from impedance data do not show any spikes on the lower frequency side indicating negligible electrode effects. A maximum conductivity of 4·5 × 10⁻⁶ S cm⁻¹ at 573 K was obtained for x = 0·8 of the Li_3−2x Al_2−x Sb _x (PO₄)₃ system.     

Synthesis and properties of magnetic solid superacid: SO4/ZrO2–B2O3–Fe3O4

A magnetic SO₄²⁻/ZrO₂–B₂O₃–Fe₃O₄ solid superacid catalyst is prepared via a simple chemical co-precipitation approach. The obtained materials were characterized in detailed by X-ray powder diffraction, thermogravimetric analysis–different scanning calorimetry, Fourier transform infrared spectroscopy (FTIR), electron microscopy (SEM and TEM), and Mossbauer spectra. Powder X-ray diffraction patterns show that in this composite oxide the transformation temperature of ZrO₂ from tetragonal to monoclinic phase is higher compared to the pristine SO₄²⁻/ZrO₂ material. The introduction of Fe₃O₄ endows the superacid with a super-paramagnetic property while in a ferromagnetic state after calcination. The superacid exhibits high catalytic activity in forming ethyl acetate by esterification.     

FeVO4/Cu3(BTC)2(H2O)3异质结制备及光催化性能

以Cu片和1, 3, 5-苯三甲酸为原料,电化学法制备经典Cu-MOF材料Cu₃(BTC)₂(H₂O)₃,即HKUST-1,作为基底金属有机框架材料(MOFs),采用室温沉积法制备FeVO₄/HKUST-1异质结复合材料,通过XRD、SEM、BET、UV-Vis DRS等对其晶体结构、形貌、比表面积、光吸收性能等进行了表征。结果表明:FeVO₄与HKUST-1复合形成异质结后,有利于光生电子-空穴的产生和转移,对目标染料污染物罗丹明B(RhB)的降解性能显著增强。可见光照射120 min后,异质结体系中RhB的降解率可达93%,而单一FeVO₄或HKUST-1体系中仅为12%和5%。此外,对材料的组成比例进行了优化,当FeVO₄与HKUST-1摩尔比为1∶1时,制备的FeVO₄/HKUST-1复合材料具有最佳的光催化性能。进一步,考察了其循环使用的稳定性,循环5次后对RhB的降解效率仍保持在90%以上,稳定性良好。      

Thermoluminescence and lyoluminescence in γ-ray irradiated and Ce3+-doped YCa4O(BO3)3 phosphors

YCa₄O(BO₃)₃ crystal having various concentration of Ce ions were synthesized by solid-state diffusion technique. XRD pattern of the sample confirmed the formation of the sample. Thermoluminescence (TL) and lyoluminescence (LL) of the γ-ray-irradiated sample were recorded. Two distinct peaks around 160 and 277 °C were observed in TL glow curves. TL intensity increased with increasing dopant concentration up to 2 mol%. A single sharp peak was observed in the LL glow curve of the sample. It was found that both TL and LL increased almost linearly with γ-ray doses up to 1.5 kGy. Photoluminescence (PL) of the sample was recorded to find the role of rare earth ion doped in YCa₄O(BO₃)₃. PL emission spectrum showed two peaks lying very close to each other around 390 nm which are characteristics of 5d → 4f transition of Ce³⁺ ions. When LL of samples was recorded after removing the TL peaks it did not show any emission. This indicates that emission centres responsible for TL are also responsible for LL.     

PEO-LiClO4-Li1.3Al0.3Ti1.7 (PO4)3复合聚合物电解质电导率

将实验室烧制的无机快离子导体盐Li_1.3Al_0.3Ti_1.7 (PO₄)₃ 、PEO 与LiClO₄ 按照EO/ Li = 8, 两种锂盐含量为变量进行复合, 通过溶液浇注法制备得到PEO-LiClO₄-Li_1.3Al_0.3Ti_1.7 (PO₄)₃ 复合聚合物电解质膜, 以示差扫描热分析法(DSC) 与电化学阻抗( EIS) 测试其性能。DSC 测试结果表明: 按照EO/ Li = 8 将Li_1.3Al_0.3Ti_1.7 (PO₄)₃ 、LiClO₄ 与PEO 复合的聚合物电解质中PEO 的结晶度由50.34 %下降到4.36 %～28.53 %。室温下该聚合物电解质所有试样的阻抗谱图在高频区呈现为压缩的半圆, 在低频区为一条倾斜的直线, 而在较高温度时, 阻抗谱图主要为一条倾斜的直线。复合聚合物电解质PEO-LiClO₄-Li_1.3Al_0.3Ti_1.7 (PO₄)₃ 的离子电导率遵从Arrhe2nius 关系, 在Li_1.3Al_0.3Ti_1.7 (PO₄)₃ 质量分数达到15 %时, 活化能最低, 即4.494425 eV, 此时电导率值最佳, 373 K时为1.161 ×10 -3 S/ cm 和298 K时为7.985 ×10-6 S/ cm。     

Crystal structure of a double Np(V) and Co(NH3)63+ maleate, Co(NH3)6[NpO2(HL)2(H2O)3](HL)2?H2O [L = OOC(HC)2COO]

Crystal structure of a double Np(V) and Co(NH₃) ₆ ³⁺ maleate Co(NH₃)₆[NpO₂(HL)₂(H₂O)₃](HL)₂H₂O [L = OOC(HC)₂COO] was studied. The crystal structure consists of complex anions [NpO₂(HL)₂(H₂O)₃]^–, HL^– anions, [Co(NH₃)₆]³⁺ cations, and water molecules of crystallization. Hydrogen bonds in which proton donors are water molecules and hexaamminecobalt cations link structural fragments to form a 3D network. The coordination polyhedra of the Np(V) atoms are pentagonal bipyramids whose equatorial planes are formed by oxygen atoms of two HL^– anions and three water molecules. Four crystallographically independent maleate anions were identified in the structure. Two of these anions enter into the Np(V) surrounding, and their coordination capacity is 1.Translated from Radiokhimiya, Vol. 46, No. 6, 2004, pp. 521–523.Original Russian Text Copyright © 2004 by Charushnikova, Krot, Starikova.     

Synthesis and characterization of Al2?xScx(WO4)3 ceramics for low-expansion infrared-transmitting windows

A low thermal-expansion material was synthesized with potential application in thermal-shock-resistant infrared-transmitting windows. The material is derived from a solid solution of Al₂(WO₄)₃, which has positive thermal expansion, and Sc₂(WO₄)₃ with a negative thermal expansion. An optimum composition of Al_0.5Sc_1.5(WO₄)₃ was identified by synthesizing solid solutions, Al_2−x Sc _x (WO₄)₃, by a solid-state route with compositions ranging from x = 0 to 2.0. A single orthorhombic phase was obtained at all compositions. A composition corresponding to x = 1.5 had a low coefficient of thermal expansion of −0.15 × 10⁻⁶/°C in the temperature range 25–700 °C. A low temperature solution combustion process was developed for this optimum composition, resulting in a single-phase powder with a surface area of ~14 m²/g and average particle size (as determined from surface area) of 92 nm. The powder was consolidated by slip-casting, sintering, and hot-isostatic pressing into visibly translucent disks with a peak in-line transmittance of 73 % at 2300 cm⁻¹. Significant infrared absorption in a 1-mm-thick disk of this material begins near 2200 cm⁻¹ and features three absorptions arising from 2-phonon transitions at 2002, 1847, and 1676 cm⁻¹. The infrared and Raman spectra are interpreted in terms of 1-, 2-, and 3-phonon vibrational transitions.     

Thermodynamic properties of (TeO2)0.95 ? n ? z(ZnO)z(Na2O)n(Bi2O3)0.05 glasses

The heat capacity (C _p ⁰) of the tellurite glasses

Elastic and inelastic properties of (Co0.45Fe0.45Zr0.1) x (Al2O3)1 ? x nanocomposites

The elastic (Young’s modulus) and inelastic (internal friction) properties of amorphous (Co₄₅Fe₄₅Zr₁₀) _x (Al₂O₃)_{100 − x} nanocomposites with various relative contents of the metallic and dielectric phases have been studied. In the region of low temperatures, the composites exhibit a peak of the internal friction (at ∼240 K), the intensity of which increases with the content of the metallic phase. For compositions above the percolation threshold, the temperature dependence of the internal friction exhibits exponential growth above 300°C, which is related to the migration of vacancy-like defects in the amorphous structure of the metallic phase.     

碳源对液相法制备Li3V2（PO4）3/C的影响

以4种不同种类的有机物(柠檬酸、水杨酸、聚丙烯酸、蔗糖)为碳源,通过液相反应合成Li3V2(PO4)3/C复合材料。研究了不同碳源对复合材料的晶型结构、形貌及电化学性能的影响。结果表明,碳源对Li3V2(PO4)3/C材料的晶型结构没有影响,但对电化学性能影响较明显,其中采用柠檬酸为碳源制得的Li3V2(PO4)3/C复合材料电化学性能最好。进一步研究了柠檬酸的加入量对复合材料的电化学性能的影响,发现当柠檬酸加入量为钒与碳的物质的量比为1∶4时,样品的平均粒径较小,电化学性能最好,0.1C首次放电比容量为123.59mAhg-1,0.5C首次放电比容量也高达117.27mAhg-1,循环10次后,仍保持在117.19mAhg-1,容量几乎没有衰减,10C时比容量仍有105.43mAhg-1。