Construction of new iodide selective electrodes based on bis(trans-cinnamaldehyde)1,3-propanediimine(L) zinc(II) chloride [ZnLCl2] and bis(trans-cinnamaldehyde) 1,3-propanediimine(L) cadmium(II) chloride [CdLCl2]

New plasticized PVC membranes iodide selective electrodes have been prepared by incorporating bis(trans-cinnamaldehyde)1,3-propanediimine zinc(II) chloride [ZnLCl2] and bis(trans-cinnamaldehyde) 1,3-propandiimine cadmium(II) chloride [CdLCl2] on the surface of graphite disk electrodes. At optimum value of variables the proposed electrodes have selective response to iodide with respect to a number of inorganic and organic anions with near-Nernstian slopes of − 60 ± 1.9 and − 58.5 ± 1.9 mV/decade of iodide concentration over the range 1.0 × 10^− 6-1.0 × 10^− 1 M with detection limits of 4.0 × 10^− 7 and 3.0 × 10^− 7 M for the electrodes based on [ZnLCl₂] and [CdLCl₂], respectively. The electrodes based on both ionophores have response times of about (6 s), with stable reproducible response during 2 months, while their responses is independent of pH over the range 2.5-10.5. The proposed electrodes successfully have been applied for evaluation of iodide ion content in real samples with complicated matrices including water and pharmaceutical samples.     

Unique electrochemiluminescence behavior of Ru(bpy)3 in a gold/Nafion/Ru(bpy)3 composite

The unique electrochemiluminescence (ECL) behavior of tris(bipyridine) ruthenium(II) (Ru(bpy)₃²⁺) immobilized in a gold/Nafion/Ru(bpy)₃²⁺ composite material was investigated. In this composite, the Ru(bpy)₃²⁺ ECL was found mainly occurred at 0-0.4 V during the cathodic scan process and the ECL peak was at about 0.1 V, which was quite different to the reported Ru(bpy)₃²⁺ ECL. Similar to the generally observed Ru(bpy)₃²⁺ ECL, the present ECL also could be enhanced by tri-n-propylamine (TPA). It is also unique that in the presence of TPA, another ECL peak at about 0.38 V occurred. These two ECL peak potentials all could be used as characteristic potential for the ECL determination of TPA.     

Reduction of Cu(II) to Cu(I) in solid CsCuCl3

The solid state reaction Cu + Cu²⁺ → 2Cu⁺ in CsCuCl₃ was studied at 499 K using a cell in which the Cu(II) sample was put between two copper discs. Mass changes, thickness of the product layer and the total electrical resistance of the cell were measured as a function of time, both with and without (spontaneous) applied voltage.     

Selective removal of Pb(II), Cd(II), and Zn(II) ions from waters by an inorganic exchanger Zr(HPO3S)2

The present study reported synthesis of a new inorganic exchanger, i.e., zirconium hydrogen monothiophosphate [Zr(HPO₃S)₂, denoted ZrPS] and its selective sorption toward Pb(II), Cd(II) and Zn(II) ions. ZrPS sorption toward all the three metals is dependent upon solution pH due to the ion-exchange nature. As compared to another inorganic exchanger zirconium phosphate [Zr(HPO₄)₂, denoted ZrP], ZrPS exhibits highly selective sorption toward these toxic metals from the background of calcium ions at great levels. Such sorption preference is mainly attributed to the presence of –SH group in ZrPS, as further demonstrated by FT-IR analysis and XPS study. Moreover, ZrPS particles preloaded with heavy metals could be efficiently regenerated with 6 M HCl for multiple use without any noticeable capacity loss. All the experimental results indicated that ZrPS is a promising sorbent for enhanced heavy metals removal from contaminated water.     

Decolourization of Methyl Orange using Fenton-like mesoporous Fe(2)O(3)-SiO(2) composite

Rapid decolourization of Methyl Orange by Fenton-like mesoporous Fe(2)O(3)-SiO(2) catalyst has been reported. The effect of various parameters such as initial pH, initial H(2)O(2) concentration, Fe content in the catalyst and initial dye concentration on decolourization process were studied. The results show that 20mg of mesoporous Fe(2)O(3)/SiO(2) composite (with Si/Fe=10) was sufficient to decolourize 0.6 mg/ml of Methyl Orange in presence of 2 ml of H(2)O(2) at an initial pH of 2.93 within 20 min. The pH range for effective decolourization (≥90%) was found to be 1-3. Leaching tests indicated that the activity of the catalyst was almost unaffected up to three consecutive cycles although ≤0.2 ppm of Fe ion was leached into treated water in each run.     

Treatment of Terasil Red R Dye Wastewater using H2O2/pyridine/Cu(II) System

The H₂O₂/pyridine/Cu(II) advanced oxidation system was used to assess the efficiency of the treatment of a 1 g L⁻¹ Terasil Red R dye solution. This system was found to be capable in reducing the concentration of chemical oxygen demand (COD) of the dye solution up to 90%, and achieving 99% in decolorization at the optimal concentration of 5.5 mM H₂O₂, 38 mM pyridine and 1.68 mM Cu(II). The final concentration of COD was recorded at 117 mg L⁻¹ and color point at 320 PtCo. Full 2⁴ factorial design and the response surface methodology using central composite design (CCD) were utilized in the screening and optimization of this study. Treatment efficiency was found to be pH independent. The amount of sludge generation was in the range of 100–175 mg L⁻¹ and the sludge produced at the optimal concentration was 170 mg L⁻¹.     

Improved photoelectrochemical detection of mercury (II) with a TiO2-modified composite photoelectrode

The spectrophotometric change of a mercury (II) (Hg²⁺) selective small molecule chemosensor has been successfully converted into a photovoltaic response upon ligating Hg²⁺. The photon excitation was followed by charge separation facilitated by TiO₂ and polyaniline (PANI), resulting in an electron transfer to an electrical back contact. The photoresponse of the Hg²⁺ selective chromophore was converted to an electron current equivalent to the amount of Hg²⁺ in solution. The favourable properties of a Hg²⁺ sensitive chemosensor was combined with the semiconductor capabilities of TiO₂ to construct a sensor that is capable of generating a current in the presence of Hg²⁺ under illumination. A composite of the fluorescent chemosensor rhodamine 6G hydrozone derivative (RS) and PANI was immobilized on indium tin oxide (ITO) plates coated with TiO₂ and subjected to photovoltammetric measurements. The photovoltammetric responses of the coated layers were investigated to determine the sensitivity and selectivity of the immobilized sensor to Hg²⁺ in the presence of background ions. The photo-response increased linearly with increasing Hg²⁺ concentration from 10 to 200 μg L⁻¹ with a limit of quantification (LOQ) of 4 μg L⁻¹. The pH independence for the photoresponse was limited by the TiO₂ layer and was optimal between pH 6 and 7.     

钌掺杂对氧化锡纳米线的光学和气敏性能的影响

采用热蒸发气相沉积法,以Au为催化剂制备了Ru掺杂SnO₂(SnO₂∶Ru)纳米线。研究了SnO₂∶Ru纳米线的晶体结构、微观形貌、光学特性和气敏性能。结果显示,纳米线具有完整的金红石结构,且表面平整。SnO₂∶Ru纳米线由O、Sn和Ru构成,它们的原子分数分别为62.60%、36.49%、0.91%。Ru掺杂引入施主型杂质能级导致SnO₂纳米线禁带宽度变窄,紫外波段的吸收系数明显增加,对丙酮、乙醇、乙二醇的气敏响应明显高于纯SnO₂纳米线,对丙酮的响应灵敏度最强。SnO₂∶Ru纳米线的最佳工作温度为210 ℃,对丙酮的响应/恢复时间短,理论探测极限为927×10-9,适合丙酮等挥发性有害气体的检测。     

暴露(001)晶面的纳米TiO2/SiC复合纤维气敏性能

锐钛矿相的TiO₂晶体主要由热力学稳定的(101)晶面组成,而具有较高活性的(001)晶面所占比例较少。通过F离子的引入,当其吸附在TiO₂的高活性(001)晶面上时,可以使晶面的表面能降低,从而制备出暴露(001)晶面的TiO₂。为提高该TiO₂的气敏性能,通过水热法将纳米TiO₂与SiC超细纤维复合,制备出具有分级结构的TiO₂/SiC复合纤维,以此解决TiO₂回收难及单晶TiO₂之间团聚的问题。结果表明,对于丙酮气体,所合成的TiO₂/SiC复合纤维的灵敏度(21.2)是暴露(001)晶面的纳米TiO₂灵敏度(14.0)的1.5倍,是商业TiO₂灵敏度(4.0)的5.3倍。     

助溶剂驱使溶胶-凝胶化SiO2/聚丙烯酸酯复合涂层

采用助溶剂和硅烷偶联剂(Z-6040)对碱性硅溶胶进行复合改性后添加到聚丙烯酸酯乳液中制备SiO2/聚丙烯酸酯杂合乳液(Si/PAE),分别考查助溶剂的种类和用量对硅溶胶的溶胶-凝胶化(sol-gel)反应及复合涂层综合性能的影响,结果发现:异丙醇是合适的助溶剂,其最佳添加量为硅溶胶质量的10%。TEM测试和纳米粒径分析发现:助溶剂可以提高无机硅颗粒在杂合乳液中的分散能力,降低Si/PAE的平均粒径。傅里叶红外光谱(FT-IR)和原子力显微镜(AFM)分析说明:Si/PAE乳液在成膜过程中,助溶剂可驱使硅溶胶发生sol-gel反应,并在涂层表面富集含硅聚合物,Si/PAE的涂层结构平整且致密。TGA分析发现:Si/PAE涂层具有较好的热稳定性。     

Preparation and characterization of Ti/SnO(2)-Sb(2)O(3)-Nb(2)O(5)/PbO(2) thin film as electrode material for the degradation of phenol

In this work, a novel electrode of titanium substrate coated with mixed metal oxides of SnO(2), Sb(2)O(3), Nb(2)O(5) and PbO(2) was successfully prepared using thermal decomposition and electrodeposition. The surface morphology and the structure of the prepared thin film were characterized by scanning electronic microscopy (SEM) and X-ray diffraction (XRD), respectively. Experimental results showed that the structure of the prepared electrode might be described as a Ti/SnO(2)-Sb(2)O(3)-Nb(2)O(5)/PbO(2) thin film and its surface was mainly comprised pyramidal-shape beta-PbO(2) crystals. The modified electrode had higher oxygen evolution potential than that of other PbO(2) modified electrodes. Electrocatalytic oxidation of phenol in aqueous solution was studied to evaluate the potential applications of this electrode in environmental science. The phenol removal efficiency in an artificial wastewater containing 0.50g/L phenol could reach 78.6% at 20 degrees C and pH 7.0 with an applied electricity density of 20mA/cm(2) and treatment time of 120min. When 21.3g/L chloride was added to this wastewater, the removal efficiency could reach to 97.2%.     

Mg(BH4)2-NaNH2体系的加热放氢性能研究

采用机械球磨法制备了Mg(BH4)2-NaNH2复合储氢材料,研究了Mg(BH4)2和NaNH2之间的相互作用及其加热放氢性能。当物质的量比为1∶2时,Mg(BH4)2与NaNH2之间发生反应:Mg(BH4)2+2NaNH2→2NaBH4+Mg(NH2)2。当物质的量比为1∶1时,Mg(BH4)2与NaNH2之间发生反应:Mg(BH4)2+NaNH2→NaBH4+MgBNH6。加热到400℃,该样品分两步进行放氢反应,放氢峰温分别在190℃和369℃,可以放出4.7%(质量分数)氢气。第一步放氢反应为MgBNH6分解产生MgH2,即:MgBNH6→MgH2+BN+2H2。第二步放氢反应为MgH2的分解:MgH2→Mg+H2。     

The gas sensitivity of nano TiO2-SnO2 film doped with Cd(II) ion

The nanocomposite oxide (0.2TiO₂-0.8SnO₂) doped with Cd²⁺ powder have been prepared and characterized by XRD and their gas-sensing sensitivity were characterized using gas sensing measurement. Experimental results show that, bicomponent nano anatase TiO₂ and rutile SnO₂ particulate thick film doped with Cd²⁺ behaves with good sensitivity to formaldehyde gas of 200 ppm in the air, and the optimum sensing temperature was reduced from 360 °C to 320 °C compared with the undoped Cd²⁺ thick film. The gas sensing thick films doped with Cd²⁺ also show good selectivity to formaldehyde among benzene, toluene, xylene and ammonia as disturbed gas and could be effectively used as an indoor formaldehyde sensor.     

Polysiloxane surface modified with bipyrazolic tripodal receptor for quantitative lead adsorption

A new silica gel compound modified N,N-bis(3,5-dimethylpyrazol-1-ylmethyl) amine (SiN(2)Pz) was synthesized and characterized by elemental analysis, FT-IR, (13)C NMR of the solid state, nitrogen adsorption-desorption isotherm, BET surface area and BJH pore sizes. The new surface exhibits good chemical and thermal stability determined by thermogravimetry curves (TGA). The effect of pH and stirring time on the adsorption of Pb(II) were studied. The process of metal retention was followed by batch method and the optimum pH value for the quantitative adsorption of this toxic metal ion was 7. At this pH value, the new functionalized polysiloxane presents further improvements and shows higher affinity (123mg of Pb(2+)/g of silica) for the effective adsorption of Pb(II) compared to others described sorbents. The extracted amounts of Pb(II) were determined by atomic absorption measurements.     

The Influence of Interface Structures on the Conducting Properties of Zirconia (ZrO2)-Based Solid Electrolytes

Zirconia-based materials are the solid electrolytes used as the principal component of solid oxide fuel cells. The present generation of fuel cell designs incorporates self-supporting thin films (80–100 m) of the electrolyte on which various coatings of electrode are applied. The operating temperature of the cell is currently in the range 800–1000°C, and understanding the interface structures associated with these structurally complex components at these temperatures remains a constant challenge. Incremental changes in conductivity brought on by interface modifications can have a large influence on the viability of any particular system for commercial application. This review outlines the influence that a number of interface structures associated specifically with zirconia-based electrolytes have on the ionic conductivity. These include grain boundary structures, structures within grains, and the influence of additives. In addition, the effect of long-term anneals on the various interfaces is addressed. In each case, the combination of ionic conductivity measurements with detailed analytical electron microscopy has provided the clues as to how the various interface structures influence the physical properties of the solid electrolyte ceramic.     

毛细微模塑和转移微模塑制备PVP/Ru(dpphen)3Cl2微图形

用毛细微模塑法和转移微模塑法分别制备了钌有机螯合物掺杂的PVP微条纹和点阵微图形。电镜照片显示,所形成的微图形很好地再现了模板的原貌,而荧光显微镜照片表明,钌有机螯合物在PVP中分散均匀。荧光光谱分析发现,分散在PVP中钌有机螯合物的发射光谱有蓝移现象。     

SiO2 layer thickness effects on the (001) texture of FePtCu:SiO2 nanocomposite films

The influence of SiO₂ layer thickness of (Fe₅₂Pt₄₈)₈₈Cu₁₂:SiO₂ multilayer nanocomposite films on their structural and magnetic properties were investigated. The films were deposited on (001) textured FePt films, and then annealed at 873 K. The crystalline texture of (Fe₅₂Pt₄₈)₈₈Cu₁₂:SiO₂ films changes drastically with respect to the thickness of the SiO₂ layers. In the film with 50-Å thick SiO₂ layers, the (111) peak was strong although the (001) orientation is dominant, and self-organized spherical FePtCu particles were formed in the SiO₂ matrix. However, in the film with 19-Å thick SiO₂ layers, flat FePt grains with perfect (001) orientation were obtained. In addition, twins with different crystalline orientations were seen in the above films with different thicknesses of the SiO₂ layers. Accordingly, different perpendicular hysteresis loops were obtained.     

Gas sensing mechanism of TiO2-based thin films

Two classes of thin film gas sensors have been studied: TiO₂ doped with Cr or Nb and TiO₂-SnO₂ mixed systems. Thin films have been prepared by the reactive sputtering from mosaic targets. It is demonstrated that titanium dioxide doped with Nb and Cr should be considered as a bulk sensor. Its performance is governed by the diffusion of point defects, i.e. very slow diffusion of Ti vacancies for TiO₂: 9.5 at% of Nb and fast diffusion of oxygen vacancies in the case of TiO₂: 2.5 at% Cr sensor. The corresponding response times are 55 min for TiO₂: 9.5 at% of Nb and 20 s for TiO₂: 2.5 at% Cr. In turn, sensors based on TiO₂-SnO₂, particularly those of the SnO₂-rich composition, belong to the group of surface sensors.     

White OLEDs based on novel emissive materials such as Zn(HPB)2 and Zn(HPB)q

Organic light emitting diodes (OLEDs) show a lot of advantages for display purposes. Because OLEDs provide white light emission with high efficiency and stability, it is desirable to apply OLEDs as an illumination light source and backlight in LCD displays. We synthesized new emissive materials, namely [2-(2-hydroxyphenyl)benzoxazole] (Zn(HPB)₂) and [(2-(2-hydroxyphenyl)benzoxazole)(8-hydoxyquinoline)] (Zn(HPB)q), which have a low molecular compound and thermal stability. We studied white OLEDs using Zn(HPB)₂ and Zn(HPB)q. The fundamental structures of the white OLEDs were ITO/PEDOT:PSS (23 nm)/NPB (40 nm)/Zn(HPB)₂ (40 nm)/Zn(HPB)q (20, 30 or 40 nm)/Alq₃ (10 nm)/LiAl (120 nm). As a result, when the thickness of the Zn(HPB)q layer was 20 nm, white emission is achieved. We obtained a maximum luminance of 15325 cd/m² at a current density of 997 mA/cm². The CIE (Commission International de l'Eclairage) coordinates are (0.28, 0.35) at an applied voltage of 9.75 V.     

Effect of precursor structure on Cu(InGa)Se2 formation by reactive annealing

Precursor structures of Mo/CuGa/In, Mo/In/CuGa, Mo/In/CuGa/In and Mo/CuGaIn were prepared on thin sodium-free glass by the sputtering of CuGa and In targets. In-situ phase evolution of precursors with temperature was investigated by a high-temperature X-ray diffraction system, which verified the existence and transformation of several intermetallics: Cu₂In, Cu₁₁In₉, Cu₃Ga, Cu₇In₃, Cu₉Ga₄ and Cu₁₆In₉ as well as elemental In. MoSe₂ layers produced during selenization were detected by scanning electron microscope and X-ray diffraction, with their thicknesses varying by precursor structure. Adhesion strength of Cu(InGa)Se₂ to each Mo layer was assessed by applying CdS chemical bath deposition process to each sample.