液液萃取-高效液相色谱-电感耦合等离子体质谱同时测定海水中的多种有机锡

利用高效液相色谱-电感耦合等离子体质谱(HPLC-ICP/MS)联用技术对海水中的五种有机锡[三甲基氯化锡(TMT)、二丁基氯化锡(DBT)、三丁基氯化锡(TBT)、二苯基氯化锡(DPhT)和三苯基氯化锡(TPhT)]进行了分离,采用Agilent TC-C18色谱柱,流动相为乙腈/水/乙酸(65∶23∶12, φ),0.05%三乙胺,pH 3.0,流速为0.6 mL·min-1, 测定了0.5～100 μg·L-1范围内五种有机锡化合物的混合标准工作曲线,其相关系数R2优于0.998,方法的检出限均小于3 ng·L-1。100 mL海水样品用10 mL含有0.2% Tropolone的CH₂Cl₂萃取两次后,有机相合并氮吹浓缩至最后一滴,加入1 mL的乙腈,用0.2 2 μm的有机滤膜过滤后分析。结果表明,海水中只检测到TPhT,含量为53.2 ng·L-1。样品的加标证明DBT, DPhT, TBT和TPhT的加标回收率均优于80%。TMT可能存在吸附或降解问题,回收率仅为50%。     

青蒿素与氯化血红素作用的荧光研究及分析应用

介绍了吡罗红为指示剂通过荧光降低法研究青蒿素与氯化血红素之间的相互作用。实验发现两者为酶和底物作用模型,作用位点为药物的过氧基团和氯化血红素活性中心的金属离子,其动力学催化常数K_m, V_max和K_cat分别为8.4×10-5 mol·L-1, 7.4×10-6 mol·L-1·s-1及50.23 s-1,催化活性分别受去激活剂和高温影响。在最佳条件下, 荧光降低值ΔF(F₀-F)与青蒿素浓度在0.0～1.27×10-6 mol·L-1范围内成线性关系, 检测限为2.3×10-8 mol·L-1, 该方法已用于测定血浆和尿液介质中的微量青蒿素。     

阴极电沉积ZnO薄膜的取向控制生长

采用阴极电沉积法,在Zn(NO3)2水溶液中,以304不锈钢为衬底制备了ZnO薄膜,研究了Zn2+浓度和电流密度对ZnO薄膜择优取向的影响规律。XRD结果表明:随着Zn2+浓度和电流密度增大,ZnO薄膜逐渐由(002)面择优取向生长转变为(101)面择优取向生长;当Zn2+浓度为0.005mol.L-1、电流密度为2.0mA.cm-2或Zn2+浓度为0.05mol.L-1、电流密度为0.5mA.cm-2时,可以得到(002)面择优取向生长的ZnO薄膜;当Zn2+浓度为0.05mol.L-1、电流密度为2.0mA.cm-2时,可以得到(101)面择优取向生长的ZnO薄膜。根据二维晶核理论,通过分析不同生长条件下的过饱和度及其对ZnO的(002)型和(101)型二维晶核形核活化能的影响,对这一规律进行了解释。可见,通过改变Zn2+浓度和电流密度能够实现阴极电沉积ZnO薄膜的取向可控生长。     

有机衬底SnO2:Sb透明导电膜的制备与特性研究

常温下,采用射频磁控溅射法在有机的柔性衬底上制备出了SnO2:Sb透明导电膜,并对薄膜的结构和光电性质进行了研究.制备的样品为多晶薄膜,并且保持了二氧化锡的金红石结构.性能良好的薄膜电阻率为6.5×10-3Ω·cm,载流子浓度为1.2×1020cm-3,霍耳迁移率是9.7cm2·V-1·s-1.薄膜在可见光区的平均透过率达到了85%. 关键词： 柔性衬底 SnO2:Sb透明导电膜 射频磁控溅射法     

快速退火对PLD法制备SnS薄膜结构和光学性质的影响

利用脉冲激光沉积(PLD)法在玻璃基片上室温生长SnS薄膜,并在Ar气保护下分别在200,300,400,500,600℃对薄膜进行快速退火处理。利用X射线衍射(XRD)、拉曼光谱仪(Raman)、原子力显微镜(AFM)、场发射扫描电子显微镜( FE-SEM)、紫外-可见-近红外分光光度计( UV-Vis-NIR)、Keithley 4200-SCS半导体参数分析仪研究了快速退火温度对SnS薄膜的晶体结构、表面形貌以及有关光学性质和电学性能的影响。所制备的SnS薄膜样品沿(111)晶面择优取向生长,退火温度为400℃时的薄膜结晶质量最好。薄膜均具有SnS特征拉曼峰。随着退火温度的升高,薄膜厚度逐渐减小,而平均颗粒尺寸逐渐增大。不同退火温度下的SnS薄膜在可见光范围内的吸收系数均为105 cm-1量级,400℃时退火薄膜的直接带隙为1.92 eV。随着退火温度从300℃升高到500℃,电阻率由1.85×104Ω·cm下降到14.97Ω·cm。     

基于荧光分析技术的大鼠肠灌流液中H_2S含量测定

荧光素汞在碱性条件下具有很强的荧光,H2S能与荧光素汞结合,使其荧光猝灭,据此建立了一种荧光法测定大鼠肠灌流液中H2S含量的方法。在0.1mol·L-1 NaOH溶液中,以Na2S作为H2S供体,荧光素汞浓度为5.0×10-5 mol·L-1,Na2S浓度为1.0×10-5 mol·L-1时,以498nm为激发波长,在522nm处测定此二元体系的荧光强度。结果表明,在4.0×10-7~2.0×10-6 mol·L-1范围内,H2S浓度与荧光强度的下降程度呈良好的负相关性,r=0.998 0,精密度实验RSD=4.59%(n=7),检出限3.5×10-8 mol·L-1,样品中H2S含量分别为1.01×10-6和1.15×10-6 mol·L-1,加标回收率为95.8%~101.0%。该方法操作简单,灵敏度高,稳定性好,可准确测定肠灌流液中H2S含量,为内源性H2S的测定提供了依据。     

氢化物-KI_3-罗丹明6G体系荧光法测定痕量硒

硒是人和动物体内必需的微量元素,但硒摄入过量会导致硒中毒,因此痕量硒的准确检测具有非常重要的意义。本研究目的是建立一种灵敏、具有选择性测定硒的氢化物发生荧光分析新方法。在0.36mol·L-1硫酸介质中,以NaBH4为还原剂,Se(Ⅳ)被还原为H2Se气体。用KI3溶液作为吸收液,I-3被H2Se气体还原成I-。当加入罗丹明6G时,罗丹明6G(Rh6G)与吸收液中的I-3形成缔合微粒导致荧光强度减弱。有Se(Ⅳ)存在时,罗丹明6G与I-3结合较少,剩余量增多,荧光强度增强。优化了分析条件,选择0.36mol·L-1 H2SO4,21.6g·L-1 NaBH4,23.3μmol·L-1 Rh6G,50μmol·L-1 KI3,激发波长为480nm时瑞利散射不影响荧光测量。在选定条件下,Se(Ⅳ)浓度在0.02~0.60μg·mL-1范围内与562nm处的荧光强度增加值ΔF呈线性关系,线性回归方程为ΔF562nm=12.6c+20.9,方法检出限为0.01μg·mL-1。考察了共存物质对氢化物发生-分子荧光法测定5.07×10-6 mol·L-1 Se(Ⅳ)的干扰情况。结果表明该法具有较高的选择性,即0.5mmol·L-1的Ba2+,Ca2+,Zn2+,Fe3+,0.25mmol·L-1的Mg2+,0.05mmol·L-1的K+,0.2mmol·L-1的Al 3+,0.025mmol·L-1的Te(Ⅵ)均对测定不产生干扰。Hg2+,Cd2+和Cu2+等易与Se(Ⅳ)结合生成沉淀,干扰Se(Ⅳ)的测定,这些干扰离子可以通过加入络合剂消除干扰。该氢化物发生-分子荧光光谱新方法已用于水中痕量硒的测定,结果满意,回收率在91.8%~107.1%之间。     

图谱分析退火对本征SnO2多晶薄膜性能的影响

提高CdTe太阳电池转换效率的有效途径之一是适当减薄CdS窗口层,减薄了的CdS层会严重影响电池性能,解决方法是在窗口层和透明导电膜之间加一层高阻本征SnO2薄膜。采用反应磁控溅射制备了具有高阻抗的本征SnO2薄膜,并对其进行了后处理,利用XRD,XPS等方法研究了退火前后薄膜的结构,成分及表面化学状态的变化。结果表明:经N2/O2=4:1气氛550℃(0.5h)退火后,样品由非晶态转变为四方相结构的多晶薄膜,具有(110)择优取向;XPS分析表明退火后薄膜的氧含量增加、O(1s)峰向低能方向移动,SnO被氧化成SnO2,使得薄膜的透过率增大,退火后的本征SnO2高阻膜非常适合作为过渡层应用于CdTe太阳电池中。     

十二烷基硫酸钠(SDS)增强若丹明6G水溶液激光激发荧光谱研究

报道了若丹明6G水溶液添加不同浓度的表面活性剂十二烷基硫酸钠(SDS)时激光激发染料的变化,发现较低的掺入量导致R6G荧光减弱,适量SDS的加入使荧光增强,在5×10-5 mol·L-1的R6G水溶液中,加入6×10-2 mol·L-1 SDS,荧光增强因子达到3.1。当R6G浓度为1×10-4 mol·L-1时,加入2×10-2 mol·L-1,染料激光阈值显著降低。测量了不同浓度的R6G溶液的吸收光谱及加入不同浓度SDS后的荧光谱,分析了不同SDS加入量下R6G荧光减弱及增强的物理机制。     

Sr-F共掺杂的SnO2基透明导电薄膜

利用离子源辅助的电子束热蒸发技术研制了高性能的Sr-F共掺杂SnO2( SFTO)基透明导电薄膜。所制备的SFTO薄膜具有良好的导电性和透过率,电阻率低于3.9×10-3Ω·cm,380~2500 nm波段的平均透过率大于85%,功函数约为5.10 eV。 SFTO透明导电薄膜为非晶态薄膜,具有较好的表面平整度( Rq <1.5 nm)。与工业上F掺杂SnO2薄膜的衬底温度(>450℃)相比,本文所用的衬底温度仅为300℃,有望直接将SnO2基透明导电非晶薄膜制备到柔性的塑料( PI、PAR或PCO)衬底上以获得性能良好的柔性电极。     

Effect of precursor concentration and bath temperature on the growth of chemical bath deposited tin sulphide thin films

SnS is a promising candidate for a low-cost, non-toxic solar cell absorber layer. Tin sulphide thin films have been deposited by chemical bath deposition technique from a solution containing stannous chloride, thioacetamide, ammonia and triethanolamine (TEA). The effects of concentration of tin salt, triethanolamine and bath temperature on the growth of tin sulphide films have been investigated in order to optimize the growth conditions to obtain tin monosulphide (SnS) films. SnS films obtained under optimized conditions were found to be polycrystalline in nature with orthorhombic structure. The optical band gap of these films was found to be 1.5 eV.     

荧光光谱研究两性表面活性剂CHAPS对钝顶螺旋藻藻胆体的解离作用

用蔗糖密度梯度高速离心的方法分离得到钝顶螺旋藻 (Spirulinaplatensis)的藻胆体 ,其室温荧光发射峰位于 6 71nm。以室温荧光光谱为表征研究了离子强度及两性表面活性剂CHAPS对藻胆体稳定性的影响。在 1mol·L-1的磷酸缓冲液中 ,藻胆体的稳定性强 ,7d内藻胆体的室温荧光发射峰位置没有变化。当用水稀释磷酸缓冲液浓度为 0 1mol·L-1,1h后藻胆体溶液的室温荧光发射峰即蓝移至 6 4 8nm ,表明藻胆体已经解离。在低浓度 (<0 6mol·L-1)磷酸缓冲液中 ,藻胆体易解离 ,解离速度随磷酸缓冲液浓度的降低而加快。在磷酸缓冲液浓度为 1mol·L-1的藻胆体的溶液中加入终浓度为 10mmol·L-1的两性表面活性剂CHAPS ,可导致藻胆体的室温荧光发射峰发生蓝移 ,说明CHAPS在高离子强度条件下也可以使藻胆体解离 ,这有利于进一步分离组成藻胆体的各种亚结构     

Tin-mono-sulfide (SnS) thin films prepared by chemical spray pyrolysis with different [S]/[Sn] ratios

SnS thin films were deposited by chemical spray pyrolysis using cost-effective and low-toxicity sources materials like tin (II) chloride dihydrate and thiourea as sources of tin and sulphur, respectively. We have studied the properties of sprayed SnS thin films with [S]/[Sn] ratios were varied from 1 to 4 in order to optimize these parameters. X-ray diffraction was used for analyzing the films structure, Raman Spectroscopy for assessing the films quality and structure, scanning electron microscope (SEM) for surface morphology and energy dispersive energy (EDS) for compositional element in samples, atomic force microscopy (AFM) for the topography of surfaces and optical spectroscopy for measuring transmittances and then deducing the band gap energies. All films obtained are polycrystalline with (111) as preferential direction for films with [S]/[Sn] ratio equals to one while for [S]/[Sn] ratios from 2 to 4 the main peak becomes (101) and the (111) peak decreases in intensity. Raman spectroscopy confirms the presence of only one SnS phase without any additional parasite secondary phases. SEM images revealed that films are well adhered onto glass surface with rounded grain. AFM confirms this result being films with [S]/[Sn] = 1 the roughest and also with the largest grain size. EDS results show an improvement of stoichiometry with the increase of the [S]/[Sn] ratio. From optical analysis, it is inferred that the band gap energy decreases from 1.83 to 1.77 eV when the [S]/[Sn] ratio changes from 2 to 4.     

Fabrication and optical properties of SnS thin films by SILAR method

Although the fabrication of tin disulfide thin films by SILAR method is quiet common, there is, however, no report is available on the growth of SnS thin film using above technique. In the present work, SnS films of 0.20 μm thickness were grown on glass and ITO substrates by SILAR method using SnSO₄ and Na₂S solution. The as-grown films were smooth and strongly adherent to the substrate. XRD confirmed the deposition of SnS thin films. Scanning electron micrograph revealed almost equal distribution of the particle size well covered on the surface of the substrate. EDAX showed that as-grown SnS films were slightly rich in tin component while UV-vis transmission spectra exhibited high absorption in the visible region. The intense and sharp emission peaks at 680 and 825 nm (near band edge emission) dominated the photoluminescence spectra.     

Preparation and properties of SnS film grown by two-stage process

SnS films have been prepared by a novel two-stage process. It involved sputtering of Sn film on glass substrate and sulfurization of the thin metallic tin precursor layers in a vacuum furnace. The X-ray diffraction results showed that the SnS layers had orthorhombic structure and (0 4 0) preferential growth is more and more obvious with the increase of sulfurization time. The SnS film obtained by this work shows high optical absorption efficiency, and the film has a direct optical band gap of about 1.3 eV. The films show p-type conductivity and the resistivity of SnS film decreased obviously under illumination.     

Preparation and characterization of electrodeposited SnS thin films

Tin sulfide (SnS) thin films have been deposited by electrodeposition using potentiostaic method on indium doped tin oxide (ITO) coated glass substrates from aqueous solution containing SnCl₂·2H₂O and Na₂S₂O₃ at various potentials. Good quality thin films were obtained at a cathodic potential −1000 mV versus saturated calomel electrode (SCE). The deposited films were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and Fourier transform infrared (FTIR). X-ray diffraction analysis shows that the crystal structure of SnS thin films is orthorhombic with preferential orientation along 〈0 2 1〉 plane. Microstructural parameters such as crystallite size, micro strain, and dislocation density are calculated and found to depend upon cathodic potentials. SEM studies reveal that the SnS films exhibited uniformly distributed grains over the entire surface of the substrate. The optical transmittance studies showed that the direct band gap of SnS is 1.1 eV. FTIR was used to further characterize the SnS films obtained at various potentials.     

Modification of structure, morphology and physical properties of tin sulfide thin films by pulsed laser irradiation

This paper presents modification of tin sulfide (SnS) thin films by pulsed laser irradiation. Tin sulfide films of 1 μm thickness were prepared using chemical bath deposition (CBD) technique. The chemical bath contained 5 ml acetone, 12 ml of triethanolamine, 8 ml of 1 M thioacetamide, 10 ml of 4 M ammonium hydroxide and 65 ml of distilled water. The chemical bath was kept at a constant temperature of 60 °C for 6 h which resulted in SnS films with 500 nm thickness. By double deposition, the final thickness of SnS thin films obtained was 1 μm. Laser processing was conducted to modify the structure, morphology and physical properties of the SnS thin films. The laser specifications were pulsed Nd:YAG laser with 532 nm wavelength, 300 mJ pulse energy and 10 ns pulse width. Properties of the laser-irradiated SnS thin films were compared with the as-prepared SnS thin films. The changes in structure, morphology, optical and electrical properties of the laser-irradiated SnS thin films were described.     

CO sensor derived from mesostructured Au-doped SnO2 thin film

Pure and Au-doped mesostructured SnO₂ thin films were successfully prepared by using non-ionic surfactant Brij-58 (polyoxyethylene acyl ether) as organic template and tin tetrachloride and hydrogen tetrachloroaurate(III) trihydrate as inorganic precursor. Thin films were deposited onto the glass substrates at 450 °C by simple spray pyrolysis technique. The novel mesostructured tin oxide thin films with different Au concentration exhibit highly selective response towards CO. The correlation of the Au incorporation in the mesostructure with particular morphology and gas sensing behavior is discussed using scanning electron microscopy (SEM), X-ray diffraction (XRD), BET surface area and transmission electron microscopy (TEM) studies.     

Effect of indium incorporation on properties of SnS thin films prepared by spray pyrolysis

Tin sulphide (SnS) thin films were deposited on glass substrate at different substrate temperature (T_s = 325 °C, 350 °C and 375 °C) by pyrolytic decomposition using stannous chloride and thiourea as precursor solutions. Also, indium-doped SnS thin films were prepared by using InCl₃ as dopant source. The dopant concentration [In/Sn] was varied from 2 at% to 6 at%. The XRD analysis revealed that the films were polycrystalline in nature having orthorhombic crystal structure with a preferred grain orientation along (1 1 1) plane. Due to In doping, the orientation of the grains in the (1 1 1) plane was found to be deteriorated. Atomic force microscopy (AFM) measurements revealed that the surface roughness of the films decreased due to indium doping. The optical properties were investigated by measuring the transmittance characteristics which were used to find the optical band gap energy, refractive index and extinction coefficient. The energy band gap value was decreased from 1.60 to 1.43 eV with increasing In concentration. The photoluminescence (PL) measurements of thin films showed strong emission band centered at 760 nm. Using Hall Effect measurements electrical resistivity, carrier concentration and Hall mobility have been determined.