低真空条件下矿物的扫描电镜能谱分析

进行矿物的X射线能谱分析时,合理地使用低真空技术可以省去矿物的喷镀过程,缩短分析时间,以及减小由样品导电性差给分析结果带来的误差。通过试验,笔者认为只要待分析的矿物粒度足够大和注意真空度的选择是可以得到满意结果的。     

PM_(10)浓度及微观特征季节分布分析——以乌鲁木齐天山区2004年为例

利用2004年乌鲁木齐城区(以天山区为例)PM10日平均浓度和气象要素观测资料,对不同季节PM10浓度变化特征、不同级别污染日数进行统计分析．同时,结合环境扫描电镜／X射线能谱(ESEM-EDX)对不同季节的颗粒物的形貌及来源进行了初步探讨。结果表明2004年PM10浓度变化为:冬季>秋季>春季>夏季;冬季出现4级以上污染日数最多,占39．5％;夏季最为洁净,好于2级的日数占到76．1％．PM10和气象因子的相关分析表明浓度与风速成正比,与降水成反比,与温度,相对湿度和逆温层厚度相关比较复杂,有时成正相关,有时呈负相关。颗粒物的形貌在不同季节特征明显,冬季颗粒物多呈圆球形,春季形貌不规则,夏季既有圆球形又有不规则形貌的颗粒,而秋季颗粒物多呈链状．     

Processing and characterization of nano-magnetic Co0.5Ni0.5Fe2O4 system

Various techniques such as X-ray diffraction (XRD), infrared (IR) spectroscopy, scanning electron micrographs (SEM), energy dispersive X-ray (EDX) and a vibrating sample magnetometer (VSM) were used to investigate the structural, morphological, and magnetic properties of spinel Co_0.5Ni_0.5Fe₂O₄ system. XRD and IR analyses enabled us to determine the functional group and structural parameters of Co_0.5Ni_0.5Fe₂O₄. EDX measurements showed the concentrations of O, Ni, Fe, and Co species involved in Co_0.5Ni_0.5Fe₂O₄ specimen from the uppermost surface to the bulk layers. The magnetization and coercivity of the as synthesized composite were 77 emu/g and 128 Oe, respectively.     

Covalent Immobilization of Tyrosinase on Electrospun Polyacrylonitrile/Polyurethane/Poly(m-anthranilic acid) Nanofibers: An Electrochemical Impedance Study

Polyacrylonitrile/polyurethane/poly(m-anthranilic acid) nanofibers were fabricated by electrospinning. Tyrosinase immobilization was performed by EDC/N-hydroxyl succinimide activation. Covalent binding of tyrosinase onto nanofibers was confirmed by Fourier transform infrared-attenuated total reflectance, and bicinchoninic acid assay revealed the amount of enzyme. Nanofiber morphology and composition were characterized by scanning electron microscopy/energy-dispersive X-ray spectroscopy (EDX). Nanofibers became smoother and thicker after tyrosinase immobilization. Effects of enzyme on nanofibers were investigated by electrochemical impedance spectroscopy and the data were fitted to equivalent electrical circuit model. EDX-mapping showed uniform distribution of enzyme. The solution resistance and charge transfer resistance of nanofibers decreased after enzyme immobilization.     

Effects of VLS and VS mechanisms during shell growth in GaAs-AlGaAs core-shell nanowires investigated by transmission electron microscopy

We investigated by means of transmission electron microscopy (TEM) the final growth stage of GaAs/AlGaAs core-shell nanowires (NWs) self-assembled by Au-catalyst assisted metalorganic vapor phase epitaxy (MOVPE). TEM observations and energy dispersive x-ray spectroscopy revealed the presence of an AlGaAs tapered region of varying chemical composition nearby the NW extreme end (i.e. between the core-shell NW trunk and the Au nanoparticle catalyst). Our findings evidence that this region exhibits an unintentional Al_yGa_1−yAs/Al_xGa_1−xAs core-shell structure, a result of the combined axial (vapor-liquid-solid, VLS) self-assembly and conventional (vapor-solid, VS) overgrowth of the material. While the VS-grown Al_xGa_1−xAs alloy retains the Al composition (x=0.3) of the AlGaAs shell along the NW trunk, the central Al_yGa_1−yAs section is made of an Al-rich (y≈0.8–0.9) alloy segment formed during AlGaAs shell overgrowth, followed by a graded-alloy segment formed upon deposition of the terminating GaAs cap layer, the latter segment due to the effect of the Al reservoir left in the Au catalyst nanoparticle (NP).     

Deionization of Coagulated,Clarified, Turbid Gauri Shankar Lake Waters by Using Ion-Exchange Technology

Abstract

Water collected from a rain fed Gauri Shankar Lake, Bhavnagar, Gujarat, India was used for this study. It was clarified by giving treatment with alum and poly aluminum chloride (PAC) to remove suspended impurities present in it. Waters having turbidity value of 100–750 NTU (Nephelometric Turbidity Units) were treated with PAC and alum. The dosage of PAC required for the treatment was 60% less as compared with alum. The clarified water was passed through columns loaded with strong acid and strong base ion-exchange resins to obtain deionized water. The experiments were carried out for 100 cycles of exhaustion and regeneration. The effect of the coagulation process conditions on ion-exchange capacity, and the physical attrition of the ion-exchange resins were studied intensively. Also, the performance of ion-exchange resins was compared with virgin ground waters from the institute's well. The resins employed in the study were subjected to EDX (Energy Dispersive X-Ray Spectroscopy) analysis to find out the presence of coagulating ions adsorbed on the resins. The resins were also subjected to SEM (Scanning Electron Microscope) analysis to find changes on their surface due to adhering materials if any.     

Grain and phase boundary segregation in WC-Co with TiC, ZrC, NbC or TaC additions

The microstructure of interfaces in WC-Co based cemented carbides with TiC, ZrC, NbC or TaC additions was analysed using energy dispersive X-ray analysis in a transmission electron microscope and using atom probe tomography. Segregation to WC/WC grain boundaries and WC/(M,W)C phase boundaries corresponding to between 0.4 and 1.2 atomic layers of close packed monolayers of Co was observed in all the materials. In addition to Co, Ti, Zr and Nb, but not Ta, segregate to the WC/WC grain boundaries. Segregation was also observed for B, P, Fe and Cr, but not Ni, to the boundaries. These are impurities that originate from the material production. Segregation of Ti, Zr, Nb and Ta to WC/binder phase boundaries was observed. If formation of a MC phase at the interface is assumed, the segregation corresponded to a thickness less than a monolayer.     

Optimizing use of the structural chemical analyser (variable pressure FESEM‐EDX raman spectroscopy) on micro‐size complex historical paintings characterization

The novel Structural Chemical Analyser (hyphenated Raman spectroscopy and scanning electron microscopy equipped with an X‐ray detector) is gaining popularity since it allows 3‐D morphological studies and elemental, molecular, structural and electronic analyses of a single complex micro‐sized sample without transfer between instruments. However, its full potential remains unexploited in painting heritage where simultaneous identification of inorganic and organic materials in paintings is critically yet unresolved. Despite benefits and drawbacks shown in literature, new challenges have to be faced analysing multifaceted paint specimens. SEM?Structural Chemical Analyser systems differ since they are fabricated ad hoc by request. As configuration influences the procedure to optimize analyses, likewise analytical protocols have to be designed ad hoc. This paper deals with the optimization of the analytical procedure of a Variable Pressure Field Emission scanning electron microscopy equipped with an X‐ray detector Raman spectroscopy system to analyse historical paint samples. We address essential parameters, technical challenges and limitations raised from analysing paint stratigraphies, archaeological samples and loose pigments. We show that accurate data interpretation requires comprehensive knowledge of factors affecting Raman spectra. We tackled: (i) the in‐FESEM?Raman spectroscopy analytical sequence, (ii) correlations between FESEM and Structural Chemical Analyser/laser analytical position, (iii) Raman signal intensity under different VP‐FESEM vacuum modes, (iv) carbon deposition on samples under FESEM low‐vacuum mode, (v) crystal nature and morphology, (vi) depth of focus and (vii) surface‐enhanced Raman scattering effect. We recommend careful planning of analysis strategies prior to research which, although time consuming, guarantees reliable results. The ultimate goal of this paper is to help to guide future users of a FESEM‐Structural Chemical Analyser system in order to increase applications.     

Improvement in corrosion resistance of commercial pure titanium for the enhancement of its biocompatibility

A new surface modification protocol encompassing an anodization treatment has been developed to improve the surface properties of biomedical titanium. Anodization in presence of nickel sulfate is one of a good way to improve the resistance of commercial pure titanium (cp‐Ti) in phosphate saline buffer solution (PSB). The potentiostatic behavior of anodized titanium in sulfuric acid with nickel sulfate differed markedly from that of titanium anodized in sulfuric acid free from nickel sulfate. Polarization and electrochemical impedance spectroscopy (EIS) recorded an increase in the corrosion resistance of the passive film. Scanning electron microscopy (SEM) and energy diffraction X‐ray (EDX) analysis were used to investigate the morphology and structure of the anodized film in absence and in presence of nickel sulfate. On the other hand, sealed anodized titanium samples exposed to PSB for up to 3 days have been studied by EIS to obtain detailed information concerning the electrochemical properties of sealed anodized titanium. An equivalent circuit that reproduces the impedance results of porous cp‐Ti oxide (TiO₂) films is proposed. These observations indicate that anodization of cp‐Ti in presence of nickel sulfate and sealing the anodized film can serve as a simple low‐temperature method to enhance the corrosion resistance of cp‐Ti when used as an implant material.