The properties of gold catalysts precursors adsorbed on the MCM-41 materials modified with Mn and Fe oxides

Silica mesoporous materials modified with manganese and iron were obtained by the hydrothermal method. Gold was introduced to pure and modified silica materials by the direct hydrothermal and impregnation methods. Nitrogen adsorption/desorption studies evidenced formation of the materials with large total surface area and mesoporous structure. Unmodified silica materials showed regular pore arrangement. The uniform porous structure was distorted in the iron or manganese containing samples. XRD, UV-Vis/DRS spectroscopy and temperature programmed reduction studies revealed changes of the nature of transition metal oxide and gold species on the different preparation stages. The oxide species after drying were strongly dispersed and partially incorporated to the silica framework. High temperature treatment led to the formation of extraframework Mn and Fe oxide species. Complex processes of gold deposition were observed during hydrothermal synthesis and impregnation of modified silica materials. The increase of the size of gold species was observed during calcination. The presence of transition metal oxides decreased sintering of gold crystallites.     

Chemical environment of copper at the surface of a CuAl2 model alloy: XPS,MEIS and TEM analyses

Air‐formed oxide on a CuAl₂ model alloy is shown to be free of copper species, with copper enriching in the alloy. With thickening of the oxide by anodizing, copper enriches further to a critical concentration at which its oxidation proceeds with incorporation of Cu(II) species into the film. Such species migrate more rapidly through the film than aluminium species. Incorporation of copper species is associated with generation of oxygen gas within the film and subsequent film rupture is due to release of the gas. Reduction of Cu(II) to Cu(I) species during XPS analysis is characterized and the accelerating role of charge neutralizing is highlighted. Copyright © 2004 John Wiley & Sons, Ltd.     

Characterization of non‐Cr‐based deoxidizers on Al alloy 7475‐T7651

The effects of three non‐chromate‐based deoxidizers, namely NaBrO₃/HNO₃, (NH₄)₄Ce(SO₄)₄/H₂SO₄ and Fe(III)/HF/HNO₃, on the Al alloy 7475‐T7651 were investigated. Several analytical methods were employed, including SEM, AES, transmission electron microscopy (TEM), electron energy‐loss spectroscopy (EELS) and glow discharge optical emission spectrometry (GDOES), to study the effects on the surface of this alloy after each treatment compared with the as‐received and alkaline‐cleaned alloy surfaces. The untreated alloy was found to have a thick oxide of 200–320 nm, consisting mainly of MgO. Alkaline cleaning results in an etching effect that thins the oxide and also deposits a thin silicate layer on the surface. In the case of the deoxidizers, there is significant removal of the native oxide of the alloy by the NaBrO₃/HNO₃ deoxidizer. There is also evidence of intermetallic attack on the alloy. The (NH₄)₄Ce(SO₄)₄/H₂SO₄ deoxidizer, which is a low‐etch‐rate deoxidizer, resulted in a slight thinning of the oxide. However, the effect was not significantly greater than with alkaline cleaning alone. The most effective deoxidizer in reducing the oxide thickness of the alloy is Fe(III)/HF/HNO₃, in which the etch rate was sufficiently high to remove completely the native oxide. In this case, equilibrium between oxide removal and the formation of new oxides on the alloy surface was achieved. Copyright © 2004 John Wiley & Sons, Ltd.     

Synthesis, single crystal X-ray analysis, and TEM for a single-sized Au11 cluster stabilized by SR ligands: The interface between molecules and particles

An SR-modified Au cluster with a sub-nanometer size, Au₁₁(S-4-NC₅H₄)₃(PPh₃)₇ (1), has been synthesized by NaBH₄ reduction of Au(S-py)(PPh₃) or by reacting [Au₉(PPh₃)₈](NO₃)₃ with HS-4-py in good yield. Its molecular structure has been elucidated by single crystal X-ray diffraction, and TEM observation has been achieved for the first time for this size of SR-modified Au clusters. The core structure is best described in terms of an incomplete icosahedron. CV measurements in CH₂Cl₂ have suggested that the cluster does not coagulate in solution with significant concentration.     

SiO2包覆纳米CaCO3的透射电镜表征

在透射电子显微镜（TEM）电子衍射模式下，用适当孔径的物镜光阑选择非晶态SiO2的衍射区域，拍摄以溶胶一凝胶法制备的SiO2包覆纳米CaCO3的暗场像。与未经包覆SiO2的纳米CaCO3的暗场像作对比，可以看出经过SiO2包覆的纳米CaCO3粒子周围有一白色亮环，从而得到SiO3包覆层的暗场照片。用高分辨方法观察了包覆层与CaCO3粒子间的界面情况。     

Synthesis and characterization of silver nanoparticle/kaolinite composites

Ag nanoparticles were synthetized in the interlamellar space of a layered kaolinite clay mineral. Disaggregation of the lamellae of non-swelling kaolinite was achieved by intercalation of dimethyl sulfoxide. The kaolinite was suspended in aqueous AgNO₃ solution and, after adsorption of Ag⁺, the ions were reduced with NaBH₄. The interlamellar space limits particle growth (d_ave=3.8–4.2 nm); however, larger silver particles may be formed on the exterior surface of kaolinite with d_ave=5.6–10.5 nm diameter. The diameter of the particles prepared in this way is depending on the initial AgNO₃ concentration. The silver nanoparticles prepared were characterized by UV–vis spectroscopy, X-ray diffraction (XRD), Small angle X-ray scattering (SAXS), X-ray photoelectron spectroscopy (XPS) and Transmission electron microscopy (TEM).     

Surface and interface characterization of polyester‐based polyurethane/nano‐silica composites

Polyester‐based polyurethane/nanosilica composites were prepared via in situ polymerization and investigated by contact angle measurement, transmission electron microscopy (TEM), atomic force microscopy (AFM) and peel testing in an Instron testing machine. The contact angle and surface free energy results show that nanosilica tended to enrich at the interface between nanocomposite polymers and the substrates, TEM indicated that nanosilica particles were evenly dispersed in the bulk and AFM demonstrated that nanoparticles were located at both the surfaces and interfaces of nanocomposite polymers and that the roughness of both the surfaces and interfaces had a decreasing tendency as the nanosilica content increased, as did the adhesion strength between the nanocomposite polymers and substrates. Copyright © 2003 John Wiley & Sons, Ltd.     

Fast heating in µ-thermal analysis</o:p>

Summary Thermal analysis of the 10 μm surface of materials using TA Instruments' μ-TA thermal probe and pulsed force mode AFM has shown promising results. This addresses the need of additional surface characterization based on principle of Thermal Analysis, which is complementary to other surface characterization techniques, i.e., Surface-IR, TOF-SIMS, etc. The method calls for identification of surface landscape by imaging first, followed by fast heating the spots of interest. The micro thermal probe is viewed to heat a small material with a tiny heater rather than to heat small material with a large heater in conventional thermal analysis. In this paper, we demonstrate the applicability in the adhesion temperature of the topical coatings of Tyvek? HDPE sheets, fusion of the heat-processed polyethylene fibers in a bundle, the surface crystallinity of PET pellets, and two examples of phase images of toughened Nylon 66. Comparisons were made where it is possible with standard thermal analysis techniques as well as with the microscopic techniques of AFM, TEM and optical.     

Thermal behavior of multiwall carbon nanotube/zeolite nanocomposites

Summary In this study we report the synthesis and thermal characterization of multiwall carbon nanotubes containing zeolite based nanocomposites. Three different zeolites (LTA, FAU and MFI) were used in this study and it was observed that the morphologies of the synthesized nanocomposites were significantly different. For FAU zeolite nanocrystals with a few nm in diameter were nucleated on the nanotubes covering their surface, however, for LTA and MFI zeolites bulky crystals with nanotubes crossing them were observed by transmission electron microscopy. One of the most important results of our study was the generation of secondary mesoporosity in the zeolites after removing the carbon nanotubes.     

超短脉冲光参量振荡器中TEM_(01)模经典增益的实现

用中心波长为850nm,重复频率为76MHz,脉宽为130fs的飞秒脉冲光产生二次谐波,泵浦TEM01模的同步光学参量振荡器,实验上获得了TEM01模大约4倍的经典增益,并给出了理论分析。这是产生高阶模飞秒脉冲光非经典频率梳的重要步骤,理论预计该增益下可以得到-2.20dB的TEM01模脉冲压缩光。