X射线荧光光谱分析

本文评述了我国在2002年7月～2004年6月间X射线荧光光谱, 包括粒子激发的X射线光谱的发展和应用, 内容包括仪器的研制、维护和维修、样品制备技术、 X射线荧光光谱基础研究、谱处理、分析方法研究和应用.     

原位变温X射线衍射测试技术及其影响因素

在X射线衍射仪中引入加热台,可以实现原位变温X射线衍射分析.原位试验是研究材料在加热或冷却过程中材料动力学的有效手段.对变温X射线衍射测试样品的要求、测量方法的原理、布鲁克D8 advance衍射仪原位变温的测试步骤以及测试过程中样品的收缩问题、背底衍射峰干扰等常见影响因素进行了详细的说明,为变温X射线衍射测试提供了具体的试验指导.     

SAPO-35分子筛的合成及其甲醇制烯烃反应性能

以六亚甲基亚胺为模板剂,采用水热法合成了不同硅含量的磷酸硅铝分子筛SAPO-35,并利用X射线衍射、X射线荧光光谱、扫描电镜、固体核磁、X射线光电子能谱和N₂吸附-脱附等方法对样品进行了表征.研究了不同硅含量的SAPO-35分子筛在甲醇转化制烯烃反应中的催化行为,同时对比分析了具有相近硅含量的SAPO-35和SAPO-34分子筛在甲醇转化反应过程中积炭物种随反应时间的演变特征,尝试将分子筛结构和其积炭失活行为进行了关联.     

Gd2O3:Eu3+ X射线溶胶-凝胶发光薄膜的制备与表征

高分辨率X射线成像系统要求其发光材料同时具有X射线截止本领强、光产额高、余辉短以及与光电器件波长匹配好等特性. Gd2O3:Eu3 因其优越的发光性能和Eu3 红光发射等优点而在高能射线激发发光材料中占有重要地位. 近几年发展起来的透明X射线薄膜发光材料具有更高的衬度和空间分辨率、热传导率、均匀性和附着力等优点[1], 因而有望成为取代传统荧光粉的新一代X射线成像材料. 在各种薄膜制备工艺中, 溶胶-凝胶法以其价格低廉、工艺简单、制备温度低、均匀性好、可实现微量掺杂等优点而日益受到人们重视, 通过该方法并辅以适当的后处理工艺可制备出透明、致密的薄膜.     

X射线荧光光谱分析

作为《分析试验室》定期评述“X射线荧光光谱分析”系列评论第八篇,本文收集国内学者在1998年7月至2000年6月期间公开发表在国内外期刊和国际会议文集上的129篇论文,并对此期间对我国X射线荧光光谱分析的概况、发展和国际上的地位进行了讲述,内容包括仪器及维修、基体校正、数据处理方法、谱分析方法的研究、标样及样品制备、全反射X射线荧光光谱、同步辐射光源X射线荧光光谱、粒子激发X射线发射、X射线荧光光谱分析方法研究及其应用。     

碳包铁负载纳米钯催化苯甲醇选择氧化

以碳包铁纳米晶(Fe@C)为载体,采用浸渍法制备了一种磁可分离的Pd/Fe@C催化剂,并运用X射线荧光光谱、透射电镜、X射线衍射和X射线光电了能谱对催化剂进行了表征,结果表明,纳米Pd颗粒的粒径分布在4～10 nm,平均粒径约为7nm,Pd物种以Pd0为主,其Pd 3d5/2结合能为335.6 eV.将该催化剂应用于苯...     

以酚醛树脂为碳源的碳改性TiO2可见光光催化剂

以合成的水溶性酚醛树脂(PF)和TiO2为原料,在N2气氛下焙烧制备了碳改性TiO2催化剂PF/TiO2,并采用X射线衍射、扫描电子显微镜、X射线光电子能谱和紫外-可见漫反射吸收光谱对样品进行了表征.结果表明,PF/TiO2催化剂具有和原料TiO2相同的晶相和形貌,且在可见光区产生明显的吸收.另外,在样品表面存在Cn,...     

短孔道Cu-Mn/Zr-Ce-SBA-15催化剂的制备及其催化甲苯燃烧性能

采用水热法制备了Zr-Ce-SBA-15(ZCS)介孔材料,并以它为载体,通过浸渍法制备了不同Cu/Mn比和Cu-Mn含量的Cu-Mn/ZCS催化剂.采用N2吸附-脱附、透射电镜、扫描电镜、X射线衍射和X射线光电子能谱(XPS)等手段对催化剂进行了表征,并在微型固定床反应器上评价了催化剂催化甲苯燃烧性能.结果表明,Cu...     

基于蒙特卡洛方法的X射线探测器能谱响应研究

为解决X射线荧光测量过程中的仪器刻度和校正难题,通过理论研究并运用蒙特卡洛方法对X射线荧光仪进行建模,得到了X射线探测器能谱响曲线。结果表明:模拟的X射线探测器能谱响应全谱与实测情况基本一致,而主成份谱线则高度一致,特征峰半高宽相对误差均在5%以内。方法为X射线荧光测量的仪器刻度和校正提供重要的研究信息,不仅为元素分析工作节省大量人力物力,也为无标样X射线荧光分析提供了有力的理论支撑。方法也可用于X射线荧光分析过程中的其他研究领域。     

D8X射线衍射仪简易变温加热台的研制

成功研制的简易变温加热台,在不更换D8X射线衍射仪的附件情况下,能快速方便的安装在衍射仪上,进行X射线衍射原位变温测试,满足了从室温至600℃的原位变温X射线衍射测试需求.更换附件时间从2~3天缩短至30 min即可进行变温X射线衍射测试,提高了测试效率.同时,节省了购买同类变温加热台近20万元的资金.     

不同形貌和尺寸的锂离子电池SnS负极材料

通过高能球磨、微波辅助合成和化学合成方法制备不同形貌和不同尺寸的SnS材料. 运用X射线衍射和透射电镜对其结构和形貌进行分析. 在透射电镜下观察发现, 所得SnS材料呈现出纳米颗粒、层片和纳米棒状. 电化学测试结果表明, 高能球磨和化学合成(无表面活性剂加入)得到的SnS材料有较好的电化学性能, 在循环40个周期后仍分别有375和414 mAh·g-1 的电化学容量. 纳米级SnS电极材料良好的电化学性能有赖于其紧凑的纳米结构, 一定的形貌及合适的尺寸. 尽管非活性相Li2S可以帮助维持SnS电极在充放电过程中的稳定结构, 但SnS的形貌及尺寸才是获得良好电化学性能的SnS电极的关键因素.     

Net-like SnS/carbon nanocomposite film anode material for lithium ion batteries

SnS particles with sizes of 5.0–6.5 nm were prepared by a facile method. Resorcinol–formaldehyde sol with addition of the as-prepared SnS nanoparticles was spin-coated on a copper foil to prepare net-like SnS/C composite thin-film electrode for lithium ion batteries after carbonization at 650 °C. The SnS/C nanocomposite thin-film electrode showed preferable first coulombic efficiency and excellent cycling stability. The discharge and charge capacities were respectively 542.3 and 531.3 mAh/g after 40 cycles. The attractive electrochemical performances were mainly ascribed to the ultra fine particle, which showed no evident aggregation in high-resolution TEM image, and the effects of 3-dimensional net-like carbon structure, which uniformly surrounded the SnS nanoparticles to guarantee the contact, acted as a buffer matrix to alleviate the volume expansion of Li–Sn alloy and provided enough paths for electrolyte to reach SnS active material during discharge–charge process.     

Synthesis and deposition of nanostructured SnS for semiconductor-sensitized solar cell

Journal of Solid State Electrochemistry - Structural, electrical, and optical properties of SnS nanoparticles and films deposited by ultrasound-assisted chemical bath were studied. The SnS was...     

Ultrasonic synthesis of In-doped SnS nanoparticles and their physical properties

Indium (In)-doped Tin (II) Sulfide (SnS) nanoparticles (NPs) were synthesized by an ultra-sonication method and their optical, electrical, dielectric and photocatalytic properties were investigated. XRD patterns of the obtained NPs indicated formation of orthorhombic polycrystalline SnS. Field emission scanning electron microscopy exhibited flower-like NPs with particle sizes below 100 nm for both SnS and In-doped SnS samples. Optical analysis showed a decrease in energy band gap of SnS NPs upon In doping. In addition, electrical results demonstrated p-type nature of the synthesized SnS NPs and enhanced electrical conductivity of the NPs due to increased tin vacancy. Dielectric experiments on SnS NPs suggested an electronic polarizations effect to be responsible for changing dielectric properties of the particles, in terms of frequency. Finally, photocatalytic experiments revealed that high degradation power can be obtained using In-doped SnS NPs.     

Enhanced electrochemical performance of SnS nanoparticles/CNTs composite as anode material for sodium-ion battery

SnS/CNTs composite as anode for SIBs exhibits high reversible capacity, good cyclability as well as rate performance, which is superior to that of pure SnS. The enhanced electrochemical performance can be attributed to the adding of CNTs as a flexible and conductive structure supporter and the formation of SnS nanoparticles with small diameter.     

Synthesis of SnS2/SnS fullerene-like nanoparticles: a superlattice with polyhedral shape

Tin disulfide pellets were laser ablated in an inert gas atmosphere, and closed cage fullerene-like (IF) nanoparticles were produced. The nanoparticles had various polyhedra and short tubular structures. Some of these forms contained a periodic pattern of fringes resulting in a superstructure. These patterns could be assigned to a superlattice created by periodic stacking of layered SnS(2) and SnS. Such superlattices are reminiscent of misfit layer compounds, which are known to form tubular morphologies. This mechanism adds up to the established mechanism for IF formation, namely, the annihilation of reactive dangling bonds at the periphery of the nanoparticles. Additionally, it suggests that one of the driving forces to form tubules in misfit compounds is the annihilation of dangling bonds at the rim of the layered structure.     

Optical and Structural Properties of Tin Sulfide Nanoparticles Obtained via Solvothermal Routes

The effect of using different solvothermal approaches, involving heat‐up and hot‐injection routes, on the phase, morphology and optical properties of tin sulfide nanoparticles using novel dibutyltin(IV) p‐methylphenyl dithiocarbamate as single source precursor compound have been studied. Dibutyltin(IV) p‐methylphenyldithiocarbamate was synthesized and characterized using various spectroscopic techniques (FT‐IR, ¹H, ¹³C and ¹¹⁹Sn), and elemental analysis. TG analysis, studied under nitrogen, revealed tin sulfide of the rare mixed‐valence binary phase (Sn₂S₃) as the final residue at the end of the decomposition process. The samples presented as SnS1 and SnS2 obtained by the heat‐up and hot injection routes respectively, at 220 °C and in the presence of oleylamine as surfactant, revealed the α‐cubic phase of SnS with Herzenbergite structure. The X‐ray diffraction analysis of the nanoparticles also revealed patterns which showed preferred growth along (111) orientation; hence, favoring anisotropic shapes which were more distinct at higher magnification images of the TEM as a pseudo spherical morphology tending toward the formation of short rods. The optical property of the nanoparticles exhibited a blue shift in the bandgap energy with respect to the bulk, which is an evidence of quantum confinement effect.     

Size and shape control of colloidally synthesized IV-VI nanoparticulate tin(II) sulfide

We report the synthesis and characterization of monodisperse SnS nanocrystals and demonstrate shape control by varying the ratio of ligands present in the reaction mixture. The nanoparticles are subsequently linked to conducting transparent substrates, and their optoelectronic response is probed. Values of the photocurrent for this system, without attempts to optimize, in the range of 6-8 nA cm(-2) were obtained.     

活性炭负载硫化锡纳米颗粒作为高效可重复使用Lewis酸催化剂催化三组分一锅法合成4H-吡喃[2,3-c]吡唑衍生物(英文)

Tin sulfide nanoparticles(SnS -NPs) were prepared in aqueous solution at room temperature on the surface of activated carbon(AC) and were investigated using field-emission scanning electron mi-croscopy(FE-SEM), transmission electron microscopy(TEM), X-ray diffraction, reflective ultravio-let-visible spectrophotometry, and spectrofluorimetry. Calculations based on the SEM and TEM images showed that the sizes of the SnS -NPs immobilized on the AC were 30–70 nm. The prepared nanocomposite was used as a heterogeneous Lewis acid catalyst for the three-components one-pot synthesis of 4H-pyrano[2,3-c]pyrazole derivatives in ethanol at 80 ℃. The reactions were efficiently performed in the presence of the prepared catalyst in short reaction times, and gave the desired products in high yields. This catalyst can be easily recovered by simple filtration and recycled up to eight consecutive times without significant loss of its efficiency.     

Preparation and electrochemical performances of carbon-coated nanoscale SnS for supercapacitors

Carbon-coated SnS as electrode materials for supercapacitor were synthesized by high-energy ball milling and following co-heating with polyvinyl alcohol. The morphology and structure of prepared carbon-coated SnS were studied by high-resolution transmission electron microscopy (HRTEM) and X-ray diffraction (XRD). Electrochemical investigation indicated that carbon-coated SnS presented preferable electrochemical performances than pristine SnS. In comparison to pristine SnS, carbon-coated SnS had better capacitive response in cyclic voltammetry and could deliver larger specific capacitance of 28.47 F/g in galvanostatical charge–discharge process. Enhanced conductivity of carbon-coated SnS revealed by Nyquist plots was considered to be responsible for its enhanced electrochemical performances.