Monodisperse carbon microspheres synthesized from asphaltene

Carbon microspheres were synthesized from asphaltene by a chemical vapor deposition (CVD) method and characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM) and Raman spectroscopy method. The results indicated the monodispersed spheres were almost curving graphitic structure with diameters from 300 to 400 nm. G mode centre of carbon microspheres had shifted upward compared with graphite. As an efficient precursor, asphaltenes were metastable structures at higher temperature. The aromatic carbon rings of asphaltenes promoted the formation of closed cage graphitic structures. The results provide a new perspective for the application of asphaltene.     

Automated chemical analysis of internally mixed aerosol particles using X-ray spectromicroscopy at the carbon K-edge

We have developed an automated data analysis method for atmospheric particles using scanning transmission X-ray microscopy coupled with near edge X-ray fine structure spectroscopy (STXM/NEXAFS). This method is applied to complex internally mixed submicrometer particles containing organic and inorganic material. Several algorithms were developed to exploit NEXAFS spectral features in the energy range from 278 to 320 eV for quantitative mapping of the spatial distribution of elemental carbon, organic carbon, potassium, and noncarbonaceous elements in particles of mixed composition. This energy range encompasses the carbon K-edge and potassium L2 and L3 edges. STXM/NEXAFS maps of different chemical components were complemented with a subsequent analysis using elemental maps obtained by scanning electron microscopy coupled with energy dispersive X-ray analysis (SEM/EDX). We demonstrate the application of the automated mapping algorithms for data analysis and the statistical classification of particles.     

NEXAFS study of multi-walled carbon nanotubes functionalization with sulfonated poly(ether ether ketone) chains

Functionalization of multi-walled carbon nanotubes (MWNTs) surface by sulfonated poly (ether ether ketone) SPEEK chains using a direct attachment reaction was investigated. A two step method was performed. MWNTs were oxidized by a nitric acid treatment to generate carboxyl groups on their surface. The grafting reaction of sulfonated groups of SPEEK with carboxyl groups present on the surface of oxidized MWNTs readily proceeds by using hexane diamine as an interlinking molecule. Transmission electron microscopy (TEM) shows that tubes are wrapped by polymer chains. Near edge X-ray absorption fine structure spectroscopy (NEXAFS) at the C K-edge, O K-edge, and N K-edge and X-ray photoelectron spectroscopy (XPS) were used to give evidence of covalent functionalization of MWNTs by SPEEK macromolecules.     

碳纤维植入犬体后的结构研究

利用Ｒａｍａｎ光谱，Ｘ射线光电子能谱和Ｘ射线衍射研究了未植入和植入犬体１．５和４．５ａ后的碳纤维，结果表明随着植入时间的延长，碳纤维表面的石墨化程度逐渐下降，但碳纤维的主体结构不变，仍为良好的石墨结构。     

X-ray absorption spectroscopy, simulation and modeling of Si-DLC films

Amorphous silicon-containing diamond-like carbon (Si-DLC) films were deposited on silicon wafers by Ar⁺ Ion Beam Assisted Deposition (IBAD) at various energy conditions. The films were examined with X-ray Absorption Near Edge Structure (XANES) spectroscopy and Extended X-ray Absorption Fine Structure (EXAFS) spectroscopy. The Si K-edge X-ray Absorption Spectroscopy (XAS) results indicate that Si-DLC films have an amorphous structure, where each Si atom is coordinated to four carbon atoms or CH_n groups. This short-range order, where a Si atom is surrounded by four C atoms, was found in all Si-DLC films. The XANES spectra do not indicate Si coordination to oxygen atoms or phenyl rings, which are present in the precursor material. A structural model of Si-DLC is proposed based on XAS findings. Simulated X-ray absorption spectra of the model produced by FEFF8 show a good resemblance to the experimental data.     

非晶碳膜中sp2和sp3相的检测方法

非晶碳薄膜由sp2和sp3杂化的碳原子组成.sp2和sp3碳原子的比例是决定非晶碳膜的结构和性能的重要参数.如何定量或定性地分析碳薄膜中sp2和sp3碳的含量一直是十分重要的问题.目前用来测定sp2和sp3碳及其比例的实验方法有13C核磁共振谱(NMR)、电子能量损失谱(EELS)、X射线光电子能谱(XPS)、椭圆偏振谱、拉曼光谱(Raman)、红外光谱(IR)等.综述了这些测定方法及其特点.     

Direct tomography with chemical-bond contrast

Three-dimensional (3D) X-ray imaging methods have advanced tremendously during recent years. Traditional tomography uses absorption as the contrast mechanism, but for many purposes its sensitivity is limited. The introduction of diffraction, small-angle scattering, refraction, and phase contrasts has increased the sensitivity, especially in materials composed of light elements (for example, carbon and oxygen). X-ray spectroscopy, in principle, offers information on element composition and chemical environment. However, its application in 3D imaging over macroscopic length scales has not been possible for light elements. Here we introduce a new hard-X-ray spectroscopic tomography with a unique sensitivity to light elements. In this method, dark-field section images are obtained directly without any reconstruction algorithms. We apply the method to acquire the 3D structure and map the chemical bonding in selected samples relevant to materials science. The novel aspects make this technique a powerful new imaging tool, with an inherent access to the molecular-level chemical environment.     

Zinc oxide epitaxial thin film deposited over carbon on various substrate by pulsed laser deposition technique

Zinc Oxide (ZnO) is a promising candidate material for optical and electronic devices due to its direct wide band gap (3.37 eV) and high exciton binding energy (60 meV). For applications in various fields such as light emitting diode (LED) and laser diodes, growth of p-type ZnO is a prerequisite. ZnO is an intrinsically n-type semiconductor. In this paper we report on the synthesis of Zinc Oxide-Carbon (ZnO:C) thin films using pulsed laser deposition technique (PLD). The deposition parameters were optimized to obtain high quality epitaxial ZnO films over a carbon layer. The structural and optical properties were studied by glazing index X-ray diffraction (GIXRD), photoluminescence (PL), optical absorption (OA), and Raman spectroscopy. Rutherford backscattering spectroscopy (RBS), scanning electron microscopy with energy dispersive spectroscopy (SEMEDS) and atomic force microscopy (AFM) were employed to determine the composition and surface morphology of these thin films. The GIXRD pattern of the synthesized films exhibited hexagonal wurtzite crystal structure with a preferred (002) orientation. PL spectroscopy results showed that the emission intensity was maximum at -380 nm at a deposition temperature of 573 K. In the Raman spectra, the E2 phonon frequency around at 438 cm(-1) is a characteristic peak of the wurtzite lattice and could be seen in all samples. Furthermore, the optical direct band gap of ZnO films was found to be in the visible region. The growth of the epitaxial layer is discussed in the light of carbon atoms from the buffer layer. Our work demonstrates that the carbon is a novel dopant in the group of doped ZnO semiconductor materials. The introduction of carbon impurities enhanced the visible emission of red-green luminescence. It is concluded that the carbon impurities promote the zinc related native defect in ZnO.     

Efficient strategy to Cu/Si catalyst into vertically aligned carbon nanotubes with bamboo shape by CVD technique

Bamboo-shaped vertically aligned carbon nanotubes (bs-VACNTs) were fabricated on Cu/Si catalyst by chemical vapour deposition (CVD) technique under the atmospheric pressure. The catalytic material (Cu/Si) played a vital role in attaining bs-VACNTs, which is synthesized by drop cast method in a cost-effective manner. Using this catalytic support, we have achieved the tip growth bs-VACNTs at low temperature with well graphitization. The as-grown carbon material was then characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), energy dispersive X-ray spectroscopy (EDX) analyzer, high-resolution transmission electron microscope (HRTEM) and Raman spectroscopy. XRD technique confirms the formation of hexagonal graphitic carbon planes of carbon nanotubes (CNTs). The surface morphology of the material was characterized by SEM, which clearly infer vertically aligned CNTs. The nature, diameter and crystallinity were noticed by HRTEM and Raman spectroscopy, respectively. Further, we have also studied the electrochemical properties of the bs-VACNTs and it seems to be proved as highly electroconductive when compared to multi-walled carbon nanotubes (MWCNTs).     

Carbon nanotubes from catalytic pyrolysis of deoiled asphalt

High purity and uniform carbon nanotubes with about 35 nm in diameter were produced by pyrolysis of deoiled asphalt in the presence of ferrocene in an atmosphere of hydrogen and argon at 1000 °C. Characterization of carbon nanotubes was carried out by field emission scanning electron microscopy (FESEM), high resolution transmission electron microscopy (HRTEM), X-ray energy dispersive spectroscopy (EDS), Raman spectroscopy and X-ray diffraction (XRD). The carbon nanotubes were highly graphitized with amorphous carbons covering the outside wall. The influence of temperature on the preparation of carbon nanotubes was also discussed.     

Hydroxyapatite–diamondlike carbon nanocomposite films

Hydroxyapatite is a bioactive ceramic that mimics the mineral composition of natural bone. Conventional plasma-sprayed hydroxyapatite coatings demonstrate poor adhesion and poor mechanical integrity. We have developed hydroxyapatite–diamondlike carbon bilayer film. The diamondlike carbon interlayer serves to prevent metal ion release and improve adhesion of the hydroxyapatite film. These films were characterized using X-ray photoelectron spectroscopy, scanning electron microscopy, transmission electron microscopy, X-ray diffraction, Raman spectroscopy, nanoindentation, and microscratch adhesion testing. Based on the results of this study, hydroxyapatite–diamondlike carbon bilayers demonstrate promise for use in several orthopedic implants.     

Improvement in hydrogen cycling properties of magnesium through added graphite

Magnesium was milled under hydrogen with three types of carbon allotropes: carbon black, graphite, and multi-walled carbon nanotubes, respectively, using a special low-energy shearing mill. Structural and phase evolution were investigated using X-ray diffractometry (XRD) and morphology was investigated by scanning electron microscopy (SEM) with energy dispersive X-ray spectroscopy (EDS). Raman spectroscopy was used to investigate the changes in the nature of carbon–carbon bonding and differential scanning calorimetry (DSC) to investigate desorption characteristics. A Sieverts-type apparatus was applied to characterize the hydrogen absorption and desorption properties. It was found that graphite not only improved the hydrogen absorption, but also the desorption kinetics.     

Characterization of cathodically deposited carbonaceous films on a silicon substrate

Carbon-based deposits were electrochemically formed on silicon substrates in ethanol at room temperature. This work was based on the work reported by Namba, who described the electrochemical deposition of diamond from organic solutions. The deposits were analysed using a scanning electron microscope, energy dispersive spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), Raman spectroscopy and electrochemical impedance spectroscopy. Scanning electron micrographs showed some crystalline deposits on the silicon. EDS was unable to identify carbon in the film, but did reveal impurities such as sodium, potassium, calcium and zinc. It was later established that the impurities most likely came from impurities in the graphite used for a counter electrode. XPS showed the presence of carbon species, and subsequently Raman spectroscopy was used to classify further the carbon deposits. Raman spectroscopy showed the presence of amorphous carbon in some films, but no diamond peak was observed for any of the films. EIS revealed that the impedance of the deposited films was nearly identical to that of the uncoated silicon, and did not resemble the impedance of diamond. Thus, in this work, carbon–based films were formed electrochemically, but these films were not diamond.     

CVD金刚石膜中黑色缺陷的存在形式

采用光学显微镜在透射光、反射光和侧光模式下研究了多晶CVD金刚石厚膜中黑色缺陷的存在形式,利用X射线光电子能谱、拉曼光谱研究了黑色缺陷的组成成分。结果表明:晶界处的裂隙或者孔洞和晶粒内部的结晶缺陷是金刚石膜内部黑色缺陷的存在形式之一。     

Charge transfer in single-walled carbon nanotubes filled with cadmium halogenides

In this work the internal channels of the single-walled carbon nanotubes (SWCNTs) were filled with cadmium chloride, cadmium bromide, and cadmium iodide by a capillary method using melts of these salts. The influence of incorporated chemical compounds on the electronic properties of the carbon nanotubes was investigated by optical absorption spectroscopy, Raman spectroscopy, near edge X-ray absorption fine structure spectroscopy, and X-ray photoelectron spectroscopy. It was found that there is the chemical bonding between carbon atoms of nanotube walls and metal atoms of encapsulated CdX₂ nanocrystals. The obtained data testify acceptor doping effect of cadmium halogenides incorporated into the SWCNT channels, which is accompanied by the charge transfer from nanotube walls to introduced substances.     

Structure and bandgap determination of InN grown by RP-MOCVD

InN thin films are grown on sapphire substrates by remote plasma-assisted metal organic chemical vapor deposition while varying the indium pulse length and substrate temperature. The effects of the indium pulse length and temperature on the structural, morphological, electronic, and optical properties of the thin films are studied. The structural parameters are determined by X-ray diffraction and X-ray photoelectron spectroscopy and the effects of incorporating oxygen atoms in the structure is described. The N K-edge X-ray absorption spectroscopy (XAS) and X-ray emission spectroscopy (XES) measurements are used to determine the band gap and it is found to be 1.80?±?0.25 eV for all samples. A complementary measurement namely, X-ray excited optical luminescence measurement is performed to confirm the band gap value obtained from XAS and XES measurements. O K-edge XAS measurements are performed to determine the presence of oxygen impurities in the samples. Meanwhile, we carry out the density functional theory calculations for Wurtzite InN, hypothetical Wurtzite-type InO_0.5N_0.5, and InO_0.0625N_0.9375 structures. We find that the measured N-edge spectra agree well with our Wurtzite InN calculations and the measured O K-edge spectra agree better with hypothetical Wurtzite-type InO_0.0625N_0.9375 than Wurtzite-type InO_0.5N_0.5.

     

Co-Ni@N-C/多孔碳复合材料的制备及电磁特性

以制备的多孔碳为基材,采用热还原法通过原位生长制备轻质化Co-Ni@N-C/多孔碳复合材料,研究了多孔碳的添加量对样品电磁波吸收性能的影响。采用X射线衍射仪(XRD)、扫描电镜(SEM)、X射线光电子能谱(XPS)、拉曼光谱(Raman)对样品的相结构、组分和微观形貌进行表征。通过矢量网络分析仪对样品在2～18 GHz频段内的电磁参数进行测试,并根据传输线理论分析了样品的电磁波吸收性能。结果表明：以多孔碳为基材制备的Co-Ni@N-C/多孔碳样品,当多孔碳含量占原材料总质量的2.7%时,样品具有良好的电磁波吸收性能,最大反射损耗值为-57.74 dB(15.12 GHz, 2.35 mm),最大有效吸收带宽为5.14 GHz(12.86～18 GHz, 2.25 mm),基本覆盖整个Ku波段。     

Studies of structural-phase state of medical titanium alloys by contemporary methods of analytical electron microscopy

An example of original studies of titanium alloys for medical applications is used to discuss methodical features of analysis of the structural-phase state of metal materials with usage of contemporary methods of analytical scanning and transmission (including high-resolution) electron microscopy. Methods of X-ray energy dispersion spectroscopy and spectroscopy of characteristic electron energy loss are described and discussed. The possibilities of these methods for local (nanometer range) measurement of concentrations of alloying elements, including light ones (carbon), are shown. An example of focused ionic beam for study of grain boundary gliding in nanostructured pure titanium at room temperature is considered.     

纳米金/单壁碳纳米管复合物的制备、表征及其多相催化的潜力

制备了一种单壁碳纳米管担载金纳米颗粒复合材料,利用X射线衍射、扫描透射显微镜、能量色散X射线分析、比表面积分析、激光拉曼光谱和紫外-可见分光光度计等对其结构进行了表征.结果表明:纳米金粒为微晶体,其平均直径为7nm且直径分布范围较窄.研究了该单壁碳纳米管担载金颗粒对仲醇的无溶剂氧化的活性和选择性,发现其转化效率可达95％.     

Preparation of diamond-like carbon films by cathodic micro-arc discharge in aqueous solutions

Diamond-like carbon films (DLC) and silicon doped diamond-like carbon films were deposited on Ni substrate by cathodic micro-arc discharge at room temperature in aqueous solutions. The deposit potential was 130 V. The structure of the films was characterized by a scanning electron microscope (SEM), X-ray photoelectron spectroscopy (XPS) and Raman spectroscopy. Raman spectra and XPS analysis demonstrated that the films were diamond-like carbon clearly. SEM observation showed that the DLC films were uniform and the thickness was about 200 nm. Potentiodynamic polarization curve indicated the corrosion resistance of the Ni substrate was markedly improved by DLC films.