SiN/bamboo like carbon nanotube composite electrodes for lithium ion rechargeable batteries

A dual stage technique employing hot filament chemical vapor deposition (HFCVD) and radio frequency sputtering was used to synthesize SiN/BCNTs (bamboo like carbon nanotubes) on copper substrates. The films were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), Electron field emission studies (EFE), charge-discharge, and cyclic voltammetry. The comprehensive characterization is consistent with a nanolayer of amorphous SiN on BCNTs. Field emission experiments confirm the excellent contact of the SiN nanolayer with the surface of the BCNTs necessary for fabrication of a coin cell. Electrochemical testing shows that SiN/BCNT electrode can deliver an initial discharge capacity of 2000 mAh g⁻¹ which is higher than the capacity of graphite and the reversible capacity after ten cycles is 300 mAh g⁻¹. The cyclic voltammetry results suggest good reversibility with Li during cycling.     

Polymer precursor synthesis of novel ZrC–SiC ultrahigh-temperature ceramics and modulation of their molecular structure

In this study, ZrC–SiC composite ceramics were prepared with varying Zr/Si molar ratios using sol–gel method. Composites were characterized by Fourier-transform infrared spectroscopy (FT–IR), X-ray diffraction (XRD), thermogravimetric analysis (TGA), transmission electron microscopy (TEM), scanning electron microscopy (SEM), Raman spectroscopy, and energy-dispersive X-ray spectroscopy (EDS). FT–IR analysis confirmed macromolecular network structure of composites, in which the precursor is composed of polyvinyl butyral (PVB) as main chain, silane molecules are interlinked via –OH moieties in PVB side chains, and Zr atoms are crosslinked with Si in corresponding proportion. Ceramic precursor begins to decompose at a temperature exceeding 1300 °C and is completely transformed into ZrC–SiC composite ceramics with corresponding Zr/Si molar ratio at 1600 °C. Raman spectroscopy and TEM results reveal that after annealing at 1600 °C, ZrC powder uniformly covers surface of SiC ceramics, and high-crystallinity graphite carbon covers ZrC powder.     

Synthesis and transport properties of La0.67Sr0.33MnO3 conformally-coated on carbon nanotubes

We report for the first time the fabrication of nanostructured ferromagnetic lanthanum strontium manganite La_0.67Sr_0.33MnO₃ (LSMO) conformally coated onto bamboo-like carbon nanotubes (BCNTs) by pulsed laser deposition. Scanning electron microscopy revealed that one-dimensional LSMO/BCNTs with diameters ranging from 100-160 nm and lengths over 10 μm were obtained. Line-scanned energy-dispersive X-ray spectroscopy profiles, selected area electron diffraction rings, and energy-filtered transmission electron microscopy maps provided further insight into the hybrid nanostructures. LSMO/BCNT and BCNT were also investigated via in situ electrical probing in a transmission electron microscope using a piezo-driven scanning tunneling microscopy holder. Modeling of the I–V characteristics of individual hybrid nanotubes yielded the resistivity, bandgap, and electron density of LSMO and BCNT. The results show that the transport properties of LSMO/BCNT are superior to those of BCNT. This research advances the integration of oxide materials and carbon nanotubes, bringing forth new avenues for miniaturization and fabrication of one-dimensional core-multishell materials with multifunctional properties that can be used as building blocks in nanodevices.     

Electrocatalytic activity of Pt nanoparticles on bamboo shaped carbon nanotubes for ethanol oxidation

Recently, bamboo shaped carbon nanotubes (BCNTs) have received increased attention for its bamboo shaped structure associated properties and its application in direct methanol/ethanol fuel cell. In this work, the potential to use BCNTs as the support material of high loaded Pt nanoparticles for improving the efficiency of ethanol/methanol fuel cell is explored. The structure and nature of the resulting Pt-BCNTS composite were characterized by transmission electron microscopy (TEM) and energy dispersive spectroscopy (EDS) spectrum, it was found that Pt nanoparticles were homogeneously dispersed on the BCNTs surfaces with 23.5% by weight. Cyclic voltammogram (CV) indicated that the Pt-BCNTs catalyst displayed excellent electrocatalytic activity and long-term stability toward ethanol oxidation. The excellent performance may be attributed to the high dispersion of nanoscale Pt catalysts and the unique nature of BCNTs. The results imply that doping N atom introduces some defective sites and active sites onto the surface of CNTs. In general, this paper demonstrates that BCNTs are promising support material for Pt-nanoparticles catalyst and can be used to enhance the efficiency of fuel cell.     

Synthesis and thermal behavior of polymeric precursors for Si?B?C?N ceramic

Polyborosilazanes (PBSZs) were synthesized by co‐ammonolysis of 2,4,6‐trichloroborazine and dichloromethylsilane and used as precursors for Si? B? C? N ceramics. The pyrolyzed products were characterized with Fourier transform infrared, X‐ray photoeletron spectroscopy, thermogravimetric analysis (TGA), X‐ray diffraction, and scanning electron microscopy (SEM). The results indicated the content of B or Si plays an important role in controlling the high temperature behavior of the precursors. The resistance of the ceramics, which were obtained from pyrolysis of PBSZs at 1500°C, toward oxidative attack up to 1000°C was also investigated by TGA and SEM/EDX. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2010     

A Novel Processing Route to Control Grain Growth in Submicrometer Alumina Compacts

A novel processing procedure for significantly suppressing grain growth in submicrometer alumina compacts has been developed and implemented with the intent of ultimately using the same processing route to control grain size in nanophase alumina compacts. In this study, partially sintered alumina pellets made from 0.5 µm starting powders are altered by the chemical infiltration of Si₃N₄. The control and infiltrated pellets are then heated to 1650°C for 4 h. The fully sintered pellets are approximately 97% dense. Suppressed grain growth is observed in the infiltrated pellets. The average grain size in the control pellets after densification is 4.2 and 1.2 µm in the infiltrated pellets. Depth of infiltration is measured using transmission electron microscopy (TEM) and scanning electron microscopy (SEM). Depending on the specific infiltration conditions used, the outer 15-50% of the infiltrated pellets exhibit a graded microstructure consisting of a region of abnormal grain growth and a region of suppressed grain growth. Abnormal grain growth is visible on the outer surfaces of the infiltrated pellets where a relatively high ratio of Si to N is present. Further into the pellet, after some depletion of the Si source gas has occurred, regions of suppressed grain growth are apparent. Based on these results, an infiltration profile is determined. A mathematical model is developed to describe the infiltration process and to determine optimal infiltration conditions. High-resolution electron microscopy (HREM), energy dispersive spectroscopy (EDS), electron energy loss spectroscopy (EELS), and X-ray photoelectron spectroscopy (XPS) are used to study the infiltrated samples.     

Effects of fluoride ion on the formation of earthworm‐like mesoporous silica

In a strong acidic environment, ordered earthworm‐like mesoporous silica has been synthesized with CTAB templating and fluoride ion (F^?) as a counterion. The synthesized products were characterized by small‐angle X‐ray diffraction (SXRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), N₂ adsorption‐desorption isotherms, and Fourier‐transform infrared spectroscopy (FTIR). The effects of F/Si mole ratio on the morphology, surface area, and the pore size of the sample were discussed. It was found that a F/Si mole ratio at 0.083 induced the formation of 3D hexagonal mesophase, whereas higher F/Si mole ratios led to the formation of 2D hexagonal mesoporous silica, the optimum molar ratio of F/Si for the formation of delicate earthworm‐like mesoporous silica was observed at 0.250. The effects of the F/Si mole ratio, surfactant chain length, acid concentration, and shear flow on morphology were also studied.     

Characterization of MHz pulse repetition rate femtosecond laser-irradiated gold-coated silicon surfaces

In this study, MHz pulse repetition rate femtosecond laser-irradiated gold-coated silicon surfaces under ambient condition were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction analysis (XRD), and X-ray photoelectron spectroscopy (XPS). The radiation fluence used was 0.5 J/cm² at a pulse repetition rate of 25 MHz with 1 ms interaction time. SEM analysis of the irradiated surfaces showed self-assembled intermingled weblike nanofibrous structure in and around the laser-irradiated spots. Further TEM investigation on this nanostructure revealed that the nanofibrous structure is formed due to aggregation of Au-Si/Si nanoparticles. The XRD peaks at 32.2°, 39.7°, and 62.5° were identified as (200), (211), and (321) reflections, respectively, corresponding to gold silicide. In addition, the observed chemical shift of Au 4f and Si 2p lines in XPS spectrum of the irradiated surface illustrated the presence of gold silicide at the irradiated surface. The generation of Si/Au-Si alloy fibrous nanoparticles aggregate is explained by the nucleation and subsequent condensation of vapor in the plasma plume during irradiation and expulsion of molten material due to high plasma pressure.     

Novel utilization of MCM-22 molecular sieves as supports of cobalt catalysts in the Fischer–Tropsch synthesis

Cobalt catalysts (2–10 wt% Co) supported on silica-rich MCM-22 zeolites have been prepared by impregnation with aqueous Co(NO₃)₂ solutions. The catalysts are characterized by X-ray fluorescence (XRF), X-ray diffraction (XRD), nitrogen adsorption, solid state nuclear magnetic resonance (NMR), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). The catalytic properties for the Fischer–Tropsch synthesis (FTS) at 280 °C, 12.5 bar and H₂/CO = 2 are evaluated. The catalysts supported on MCM-22 exhibit the highest selectivity to long-chain (C₅₊) hydrocarbons when MCM-22 supports are synthesized with the appropriate Si/Al ratio.     

Residual stress relief of hard a-C films though buckling

To characterize the adhesive failure mode in amorphous-carbon (a-C) films, and to explore the effects of stress relief mechanism on the mechanical properties of the films, the microstructure and the morphologies of the buckled and peeled a-C films were characterized by various techniques, including transmission electron microscopy (TEM), scanning electron microscopy (SEM), Raman spectrum and X-ray photoelectron spectroscopy (XPS). Results indicated that there is obvious buckling between the stress relieved a-C films and Si substrates, and the development of the buckling blister was derived from the residual compressive stress. The as-deposited a-C films voluntarily buckled along the film growth direction above Si substrate when film thickness reached a certain size, and became more and more remarkable, resulting in eventual peeling. These buckling and peeling processes can relieve the residual stress of the a-C films by eliminating the mechanical restriction of Si substrates. The corresponding sp² hybridization transformation and the reconfiguring graphitic phase were detected in the stress relived a-C films, which can induce buckling and spalling in the a-C films.     

Copolymerization of amine-containing monomers and dodecyl (meth)acrylate in toluene: controlling compositional heterogeneity

This study focuses on a facile approach to create polyelectrolyte/SiO₂ composite thin films. The film was fabricated by alternate deposition of N-[3-(trimethoxysilyl)propyl]diethylenetriamine (C₁₀H₂₇N₃O₃Si, TPDT in short) and poly(acrylic acid) (PAA). The layer-by-layer assembly process was accompanied by sol–gel transition of TPDT. The resultant films were investigated in detail by Fourier transform infrared spectroscopy (FT-IR), UV-Visible spectroscopy (UV–vis), ellipsometry, thermogravimetric analysis (TGA), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The results indicated that the films grew exponentially with increasing bilayer number. During deposition, hydrolysis and condensation of silanol groups in the film resulted in the formation of a Si-O-Si network embedded into the framework of the polymer. The obtained free-standing films had high transparency even with a high content of silica, and showed good mechanical properties with a tensile strength of 32.8 MPa at break.     

Electrochemical and morphological assessments of inhibition level of 8-hydroxylquinoline for AA2024-T4 alloy in 3.5% NaCl solution

The corrosion inhibition of AA2024-T4 in 3.5% NaCl solution by 8-hydroxylquinoline (8-HQ) was investigated by potentiodynamic polarisation (PDP), electrochemical impedance spectroscopy and dynamic electrochemical impedance spectroscopy. Experimental results were supported with scanning electron microscopy (SEM), atomic force microscopy and Fourier transform-infrared (FTIR) spectroscopy analysis. It was found that 8-HQ molecules adsorbed on the alloy surface and protected it against corrosion. SEM, energy dispersive spectroscopy, and FTIR results confirm the adsorption of 8-HQ molecules on AA2024-T4. The inhibition efficiency of 8-HQ is found to increase with increase in concentration and the highest concentration studied (0.05 M) offered corrosion inhibition efficiency of 84%. PDP results show that 8-HQ acts as mixed type inhibitor in the studied medium.     

Characteristics of vanadium-substituted mesoporous silica with wormhole framework structure: effects of vanadium content

Vanadium-substituted wormhole framework structure (V-WMS) mesoporous silicas (V-WMS) with various Si/V ratios in the range of 15 and 200 were prepared at ambient temperature by neutral surfactant templating pathway. The materials were synthesized by using dodecylamine as a template and tetraethylorthosilicate as a silicon source. They were characterized by energy dispersive X-ray spectroscopy (EDS), powder X-ray diffraction (XRD), N₂ adsorption–desorption, thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier-transform infrared absorption spectroscopy (FT-IR) and ultraviolet-visible absorption spectroscopy. V-WMS samples shown characters of larger framework wall thickness, small crystallite domain sizes, and complementary textural mesoporosities in comparison with M41S materials. These mesoporous V-WMS samples exhibited irregularly shaped mesoscale fundamental particles which aggregated into larger particles. They also demonstrated better thermal stability than MCM-41. An absorption band of FT-IR at ca. 960 cm⁻¹ was assigned to the vibration of Si–O–V linkages. These samples also showed one strong UV–visible absorbance with overlapping maxima at about 255 nm. The results show that vanadium was incorporated into the structure of wormhole mesoporous silica (WMS). However, for V-WMS with high vanadium content (Si/V < 25), a broad shoulder in XRD pattern was observed at about 3–4°, suggesting the presence of impurity phase of vanadium species in the sample. The efforts in preparing V-WMS specimens by neutral-template synthesis route had led to new mesoporous silica molecular sieves with catalytically active vanadium centers.     

热解温度对牡蛎壳物理化学特性的影响

采用程序升温热解技术研究牡蛎壳煅制过程。通过运用X 射线衍射（XRD）、扫描电子显微镜（SEM）、红外光谱（FTIR）、能谱仪（EDS）和热重（TG）等表征技术手段,分析研究高温煅制前后牡蛎壳的物理化学特性变化规律。研究表明,在445℃附近牡蛎壳中的碳酸钙由文石型相转变方解石型,756.2℃处最大热失重速率为5.24%min?1,是方解石型碳酸钙分解所致。800℃高温煅烧后碳酸盐分解产生的CaO具有较强的吸水能力生成Ca(OH)2,高温煅制过程对牡蛎壳中Si有明显的富集作用。     

EDTA-assisted template-free synthesis and improved photocatalytic activity of homogeneous ZnSe hollow microspheres

Homogeneous ZnSe hollow microspheres were synthesized on a large scale through an EDTA-assisted mixed solvothermal strategy without any surfactants and templates. The as-synthesized ZnSe microspheres were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), and UV–vis absorption spectroscopy. The results of photodegradation of methylene blue (MB) indicate that the hollow microspheres exhibit a visible-light-responsive photocatalytic behavior. As compared with the bulk ZnSe, the photocatalytic efficiency for the hollow microspheres was enhanced remarkably, which might be related with the hollow aggregates of ZnSe nanocrystallites.     

Crystalline structure of YSZ thin films deposited on Si(111) substrate by chemical vapor deposition

Yttria-stabilized zirconia (YSZ) thin films were formed on Si(111) substrate by chemical vapor deposition (CVD) in a temperature range of 650–800 °C using β-diketone metal chelates. The scanning electron microscopy (SEM) and X-ray diffraction (XRD) data evidenced that YSZ thin films have a smooth surface with fine grains and crystalline structure, respectively. The crystalline structure of YSZ films was affected by the deposition temperature. The X-ray photoelectron spectroscopy (XPS) data indicated that the YSZ film grows thick enough to prevent the diffusion of Si.     

纳米纤丝化纤维素制备及硅烷化改性

以脱脂棉为原料, 高压均质法制备纳米纤丝化纤维素(NFC), 并以三甲基氯硅烷和十八烷基三氯硅烷为改性剂,分别对NFC进行硅烷化改性。采用透射电子显微镜(TEM)、傅里叶变换红外光谱(FT-IR)、X射线衍射光谱(XRD)、扫描电子显微镜(SEM)对NFC和硅烷化改性NFC的超微形貌和结构等进行表征。研究结果表明NFC超微形貌呈纤丝状, 直径尺寸大多为20 nm, 长度尺寸主要分布在500~1 000 nm, 结构为纤维素Ⅰ型;FT-IR和SEM分析结果表明所制备的硅烷化改性NFC中, 150 μL三甲基氯硅烷改性NFC的改性效果较好, 其超微形貌呈纤丝状。     

Covalent grafting of polyacrylamide onto mesoporous MCM-41 silica via free radical polymerization

MCM-41 mesoporous silicas were covalently modified with polyacrylamide (PAAm) by a novel grafting strategy. The effect of various parameters such as monomer concentration, reaction time, and temperature on the content of PAAm onto MCM-41 silicas were studied. Modified silicas were characterized by X-ray diffraction (XRD), infrared spectroscopy, FT-IR, thermogravimetric analysis, nitrogen adsorption–desorption analyses, scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray photoelectron spectroscopy which confirmed the grafting process. According to XRD, SEM and TEM results, PAAm-modified MCM-41 silica did not show changes in its morphology and mesostructure by comparing with pristine MCM-41. Nitrogen adsorption–desorption studies showed that the attaching of PAAm onto MCM-41 silica decreased the values of pore size, pore volume and surface area.     

Porous silica supported Co2+-tetrachlorophthalocyanine (CoPcCl-APTES@SiO2): a novel and recyclable organic–inorganic hybrid catalyst for eco-friendly oxidation of secondary alcohols

A novel, selective and recyclable cobalt based catalyst has been synthesized by covalent grafting of Co²⁺-tetrachlorophthalocyanine (CoPcCl) onto porous silica functionalized with 3-aminopropyltriethoxysilane (APTES), and the resulting organic–inorganic hybrid porous material was found to be highly effective catalyst for peroxidative oxidation of secondary alcohols. The porous material was characterized by elemental analysis, diffuse reflectance UV–Visible spectroscopy, ¹³C CPMAS and ²⁹Si CPMAS NMR spectroscopy, X-ray diffraction (XRD), Scanning electron microscopy (SEM), BET surface area analysis, Energy dispersive X-ray fluorescence (ED-XRF), Fourier transform Infrared (FT-IR) and Atomic absorption spectroscopy (AAS) techniques. High turnover frequency, mild reaction conditions, high selectivity for ketones, and easy recovery and reusability of the catalyst renders the present protocol highly essential to address the industrial needs and environmental concerns.     

Sonochemical preparation of palygorskite nanoparticles

Palygorskite nanoparticles were prepared by sonochemical reaction. The products were characterized by X-ray fluorescence analysis (XRF), X-ray powder diffraction (XRD), thermal gravimetry analysis (TGA), differential thermal analysis (DTA) and infrared spectroscopy. The morphology and size of the nanorods were observed by scanning electron microscopy (SEM) and transmission electron microscopy (TEM).