Structural colors and physical properties of elytra in the jewel beetle,Chrysochroa fulgidissima,using surface analytical techniques

Structural coloration frequently originates from the interaction of light with multilayers of thin films in living organisms. One example where structural colors are created by multilayers is the jewel beetle, Chrysochroa fulgidissima, which has highly iridescent green elytra with longitudinal red stripes. We examine the structure, chemical information, and physical properties of the epicuticle of the jewel beetle by using atomic force microscopy (AFM), scanning electron microscopy (SEM), transmission electron microscopy (TEM), nanoindentation, and time-of-flight secondary ion mass spectrometry (ToF-SIMS). AFM and SEM were used to analyze the surface structures of the green elytra and red stripes of the jewel beetle's wing. SEM and TEM images obtained from the cross-sectioned cuticle samples of green and red areas indicated that the color arises from interference reflectors and reflectors consist of successive repeating layers of different electronic densities. Nanoindentation results showed that the green area of the elytron possesses a higher hardness and reduced modulus compared with the red area. To analyze the surface of the elytra and to compare multilayers of the green area with those of the red area, mass spectra and depth profiles were acquired by ToF-SIMS with C₆₀ and Ar cluster ion beams. The epicuticle consists of several layers with alternating high and low abundances of inorganic and organic fragment ions, with approximately 16 layers in the green and 12 layers in the red area. Therefore, ToF-SIMS combined with other analytical techniques indicate that multilayer reflection is a major mechanism of the jewel beetle's iridescence causing structural coloration.     

Microscopic study of ultra-thin gold layers on polyethyleneterephthalate

Continuous and discontinuous gold layers sputtered on polyethyleneterephthalate (PET) were characterized using atomic force microscopy (AFM), scanning electron microscopy (SEM) and by reflection of microwave radiation. The changes in the surface morphology of the continuous and discontinuous gold layers as a function of the sputtering time were clearly observed by AFM technique. SEM imaging of very thin gold layers was adversely affected by specimen charging. For medium sputtering times, when a continuous gold coverage is already formed, the SEM technique still show the presence of regions with very thin gold coverage which gradually disappear at longer sputtering times. Both, the AFM and SEM techniques confirmed that in the course of the gold deposition the initially small gold clusters grow and finally associate in a continuous layer. It was shown that the sub-microne metallic structures could be modeled by artificial, significantly larger structures prepared on PET by lithographic etching.     

Characterization of DNA Layers Adsorbed on Glassy Carbon Electrodes

A DNA layer adsorbed at glassy carbon electrodes (GCE) was characterized by ellipsometry, atomic force microscopy (AFM) and scanning electron microscopy (SEM). The presence of the adsorbed DNA layer on polished glassy carbon electrodes was assessed indirectly by ellipsometric measurements. Ellipsometry was also useful to evaluate the influence of the oxide layer formed on glassy carbon electrodes, either spontaneously or after electrochemical pretreatments, on the DNA adsorption and further electrooxidation process. SEM and AFM images of the electrode surface covered by a thick layer of DNA reveal a nonuniform distribution, leaving channels and islands of the biological material.     

尼龙66-盐与碳纤维复合-固态缩聚的研究

本工作借助偏光显微镜,扫描电子显微镜和热分析方法(DSC,TGA)研究了尼龙66盐与碳纤维复合-固态缩聚反应历程及纤维-树脂之间的界面效应。发现对尼龙66盐的“原位固态缩聚”存有如碳纤维表面的成核结晶和催化效应之类的界面效应。讨论了碳纤维的界面效应对尼龙66基体的外延结晶和熔融行为及其热氧化稳定作用的影响。     

Preparation and characterization of coaxial electrospun thermoplastic polyurethane/collagen compound nanofibers for tissue engineering applications

Collagen functionalized thermoplastic polyurethane nanofibers (TPU/collagen) were successfully produced by coaxial electrospinning technique with a goal to develop biomedical scaffold. A series of tests were conducted to characterize the compound nanofiber and its membrane in this study. Surface morphology and interior structure of the ultrafine fibers were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM) and atomic force microscopy (AFM), whereas the fiber diameter distribution was also measured. The crosslinked membranes were also characterized by SEM. Porosities of different kinds of electrospun mats were determined. The surface chemistry and chemical composition of collagen/TPU coaxial nanofibrous membranes were verified by X-ray photoelectron spectroscopy (XPS) and Fourier transform infrared spectrometry (FTIR). Mechanical measurements were carried out by applying tensile test loads to samples which were prepared from electrospun ultra fine non-woven fiber mats. The coaxial electrospun nanofibers were further investigated as a promising scaffold for PIECs culture. The results demonstrated that coaxial electrospun composite nanofibers had the characters of native extracellular matrix and may be used effectively as an alternative material for tissue engineering and functional biomaterials.     

Analysis of AlGaAs/GaAs superlattices by means of sputter-assisted AES,SEM and TEM

This paper reports the developments of evaluation methods on epitaxially grown superlattices by means of sputterassisted Auger electron spectroscopy (AES), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). AlGaAs/GaAs semiconductor superlattics were grown epitaxially by metal–organic chemical vapour deposition (MOCVD). The layer thickness of the superlattices ranged from a few to ten nanometers. Firstly, developments of Auger depth profiling were tried by using: (1) a differential pumping-type ion gun instead of a static pressure type to reduce the oxygen adsorbates on the AlGaAs layer; (2) low-energy Auger signals instead of high-energy ones to shorten the escape depth; and (3) the lowest ion etching energy of 0.2 keV instead of 1 keV to reduce the surface roughening effects. It is shown that the depth resolution of sputter-assisted AES is attainable to 1.5 nm. Secondly, high-resolution SEM can be used as an easy evaluation method by observing the cleaved surface of superlattices, since the layers can be distinguished by signal contrast. Also, TEM can be used as an evaluation method by observing the (110) cross-section thinned sample. The dark field image has a high contrast between AlGaAs and GaAs using the (002) diffraction. It is confirmed from these AES, SEM and TEM evaluations that the hetero-interface abruptness of AlGaAs/GaAs superlattices grown by MOCVD is of the order of one monoatomic layer.     

聚醚醚酮/碳纤维复合材料的界面结构以及结晶形态的研究

本文采用扫描电子显微镜观察经氩等离子刻蚀后PEEK/碳纤维复合材料的界面层结构和PEEK树脂的结晶形态。无论是从熔体还是从橡胶体结晶,PEEK树脂的结晶都是从碳纤维表面诱导开始,最后形成横穿晶体结构。在高碳纤维含量的复合材料中,PEEK的球晶尺寸主要由碳纤维之间的距离控制,受温度的影响较小。在PEEK/碳纤维复合材料的结晶过程中,第一片晶片在碳纤维表面取向生长方式为:晶体的ā轴(厚度方向)平行于维纤径 向。b轴(晶片生长方向)与纤维最小圆截面的切线重合,(?)轴(垂直晶片平面的方向)平行于纤维轴向。由于球晶成核过程是取向生长,因而生成的球晶也按一定的方式取向。     

重离子径迹模板法合成银纳米线

聚碳酸脂(PC)膜被高能重离子辐照后沿入射离子路径产生潜径迹, 把带有潜径迹的膜经紫外光敏化后置于NaOH 溶液中进行蚀刻, 通过选择蚀刻条件, 在PC 膜内得到直径从100 到500 nm 导通的核径迹孔. 以带有核径迹孔的PC 膜为模板, 用电化学沉积法制备出不同直径的银纳米线. 在特定的实验条件下(沉积电压25mV、电流密度1-2 mA·cm-2、温度50 益和电解液为0.1 mol·L-1的AgNO3溶液), 获得了沿[111]方向择优取向生长的具有单晶结构的银纳米线. 利用扫描电子显微镜(SEM)、X射线衍射(XRD)、透射电子显微镜(TEM)及选区电子衍射(SAED)等手段对银纳米线的形貌和晶体结构特征进行了表征.     

Characterization of the morphology of co-extruded, thermoplastic/rubber multi-layer tapes

Tapes with alternating semi-crystalline thermoplastic/rubber layers with thicknesses varying from 100 nm up to several μm were prepared by multi-layer co-extrusion. The variation in layer thickness was obtained by varying the thermoplastic/rubber feed ratio. A systematic study on the use of various microscopy techniques to visualize the morphology of the layered systems is presented. The relatively large length scales and the sample preparation make optical microscopy (OM) unsuitable to study the morphology of the multi-layer tapes. Although excellent contrast between the thermoplastic and rubber layers can be obtained, the usually applied, relatively large magnifications limit the use of transmission electron microscopy (TEM) and atomic force microscopy (AFM) to small sample areas. The large range of applicable magnifications makes scanning electron microscopy (SEM) the most suitable technique to study the morphology of the multi-layer tapes. The sample preparation for SEM with a secondary electron (SE) detector is often based on the removal of one of the components, which may induce changes in the morphology. SEM with a back-scattered electron (BSE) detector is a very convenient method to study the morphology over a wide range of length scales, where the contrast between the different layers can be enhanced by chemical staining. Finally, the nucleation behavior (homogeneous versus heterogeneous) of the semi-crystalline layers, as probed by differential scanning calorimetry (DSC), provides valuable information on the layered morphology. The use of relatively straightforward DSC measurements shows a clear advantage with respect to the discussed microscopy techniques, since no sample preparation is required and relatively large samples can be studied, which are more representative for the bulk.     

Structural characterization of a spin-assisted colloid-polyelectrolyte assembly: stratified multilayer thin films

The assembly of polyelectrolytes and gold nanoparticles yields stratified multilayers with very low roughness and high structural perfection. The films are prepared by spin-assisted layer-by-layer self-assembly (LbL) and are characterized by X-ray reflectivity (XRR), UV-vis spectroscopy, atomic force microscopy (AFM), and transmission electron microscopy (TEM). Typical structures have four repeat units, each of which consists of eight double layers (DL) of poly(sodium 4-styrenesulfonate)/poly(allylamine hydrochloride), one monolayer of gold nanoparticles (10 nm diameter), and another layer of poly(allylamine hydrochloride). XRR scans show small-angle Bragg peaks up to seventh order, evidencing the highly stratified structure. Pronounced Kiessig fringes indicate a low global roughness, which is confirmed by local AFM measurements. TEM images corroborate the layered structure in the growth direction and nicely show the distinct separation of the individual particle layers. An AFM study reveals the lateral gold particle distribution within one individual particle layer. Interestingly, the spin-assisted deposition of polyelectrolytes reduces the roughness induced by the particle layers, leading to self-healing of roughness defects and a rather perfect stratification.     

Multiple hydrogen bonding induced self-assembly: transformation from nanofibrils to nanosphere with aromatic oligoamide incorporated polyethylene glycol

Aromatic oligoamides bearing six potential hydrogen-bonding sites were designed and synthesized. Functionalized with two polyethylene glycol (M_w?=?2000), this aromatic oligoamide could self-assemble via hydrogen bonds to form nanofibrils in nonpolar solvents as a result of aggregation. The resulting aggregates were characterized by scanning electron microscopy (SEM) and atomic force microscopy (AFM) and dynamic light scattering (DLS). Upon adding another aromatic oligoamide containing complementary hydrogen bond donors and acceptors, transformation from nanofibrils to nanosphere was observed due to formation of hydrogen-bonded duplex. The nanospherical micelle was corroborated by SEM, transmission electron microscopy (TEM) and AFM tests. The results achieved here demonstrate an alternative route to effect supramolecular structures via multiple hydrogen bonding-induced self-assembly process.     

Layered nanoparticles modified by chain end functional PE and their nanocomposites with PE

Layered materials (MMT,LDH) were successfully modified by chain end functionalized polyethylene via an ion exchange method.The samples were characterized by using elemental analysis,Fourier transform infrared (FTIR) spectrum,X-ray diffraction (XRD),scanning electron microscopy (SEM),transmission electron microscopy (TEM) and thermogravimetric analysis (TGA).The XRD results demonstrated that MMT was successfully exfoliated with the disappearance of [001] peak.For the LDH,the peak [003] moved to a low angle and greatly weakened,indicating that LDH was successfully functionalized and completely intercalated or exfoliated.HDPE/layered nanocomposites were obtained between HDPE and different content of functional layered materials.The SEM and TEM results of nanocomposites showed the layered materials were well dispersed in the HDPE matrix,with a particle size of 100-200 nm.     

Supramolecular self-assembly of block copolymer based on rigid surfactant

The supramolecular self-assembling of pyridine-containing amphiphilic block copolymers (PS-b- P4VP and PS-PI-P2VP) and 4-biphenylcarboxylic acid (BPCA) in selective solvents has been systematically studied. BPCA molecules are able to complex with the vinylpyridine (VP) moieties through hydrogen bonding, which leads to a transformation of spherical block copolymer micelles into structured nanofibers in solutions. The effects of molar ratio of BPCA to the VP repeat units, solvent selectivity, and copolymer composition on the supramolecular complex nanofiber formation have been systematically investigated by atomic force microscopy (AFM), transmission electron microscopy (TEM), and scanning electron microscopy (SEM). The formation mechanism of supramolecular self-assembly nanofibers was discussed.     

Comparative study of nanoscale surface structures of calcite microcrystals using FE-SEM, AFM, and TEM.

The bulk morphology and surface features that developed upon precipitation on micrometer-size calcite powders and millimeter-size cleavage fragments were imaged by three different microscopic techniques: field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM) of Pt-C replicas, and atomic force microscopy (AFM). Each technique can resolve some nanoscale surface features, but they offer different ranges of magnification and dimensional resolutions. Because sample preparation and imaging is not constrained by crystal orientation, FE-SEM and TEM of Pt-C replicas are best suited to image the overall morphology of microcrystals. However, owing to the decoration effect of Pt-C on the crystal faces, TEM of Pt-C replicas is superior at resolving nanoscale surface structures, including the development of new faces and the different microtopography among nonequivalent faces in microcrystals, which cannot be revealed by FE-SEM. In conjunction with SEM, Pt-C replica provides the evidence that crystals grow in diverse and face-specific modes. The TEM imaging of Pt-C replicas has nanoscale resolution comparable to AFM. AFM yielded quantitative information (e.g., crystallographic orientation and height of steps) of microtopographic features. In contrast to Pt-C replicas and SEM providing three-dimensional images of the crystals, AFM can only image one individual cleavage or flat surface at a time.     

Application of surface analysis in study on removal mechanism and abrasive selection during fused silica chemical mechanical polishing

In this work, surface analysis technology is employed to investigate the removal mechanism and the selection of abrasive during fused silica chemical mechanical polishing (CMP). Morphology of abrasives is inspected by scanning electron microscope (SEM). The atomic force microscope (AFM) is used to determine the surface roughness (Rq) and undulating (PV) of the polished fused silica surface. The results show that abrasive morphology has a tremendous influence on removal rate (MRR) and PV but has little effect on the Rq. The AFM and infrared spectroscopy (IR) analysis show that a soft layer, called “silica gel membrane (SGM),” existed on the polished surface is the critical reason for the differences of MRR, Rq, and PV during CMP. For three kinds of micro-ceria abrasives, the abrasive with a rougher surface gets more opportunities to contact the surface of fused silica, yielding higher MRR. Regarding different kinds of nano-abrasives, there are more SGM induced by nano-ceria abrasive resulting from higher chemical reaction rate. The element contaminations on the polished fused silica have been assessed using X-ray photoelectron spectroscopy (XPS), and the results suggest that there are depths of 3.6 and 5.4-nm element contaminations on the polished surface of fused silica with nano-ceria and nano-alumina abrasives, respectively. While the surface polished by nano-silica is free of heterogeneous element contaminations. Based on study results, a novel polishing slurry is designed by modifying the chemical composition of nano-silica. Comparing with ceria-based slurry, the silica-based slurry has better removal efficiency, and surface quality in fused silica precision machining.     

Gold Nano Particle and Reduced Graphene Oxide Composite Modified Carbon Paste Electrode for the Ultra Trace Detection of Arsenic (III)

Gold nanoparticles (AuNPs) and reduced graphene oxide (RGO) composite modified carbon paste electrode (CPE) was prepared by electrodepositing AuNPs over the reduced graphene oxide (RGO) modified carbon paste electrode. The composite material was characterised using scanning electron microscopy (SEM) and transmission electron microscopy (TEM) and atomic force microscopy (AFM) techniques. The nano composite modified electrode was applied for the determination of total As and for the inorganic speciation of As(III) and As(V) in environmental samples. The linear dynamic range was obtained for the determination of As(III) in the present method from 1μgL⁻¹ to 20 μgL⁻¹ and the limit of detection(LOD) in the standard solution was found to be 0.13 μgL⁻¹ for the 300 sec deposition time in 10 mL supporting electrolyte solution. This method was applied for the determination of As (III) in water and soil samples. The results were agreed well with the result obtained from the hydride generation atomic absorption spectrometry.     

Focused ion beam sectioning and lift-out method for copper and resist vias in organic low-k dielectrics.

The focused ion beam lift-out technique for scanning electron microscope (SEM) and transmission electron microscope (TEM) sample preparation was shown to be applicable to copper/low-k dielectric semiconductor technology. High resolution SEM, TEM, and scanning transmission electron microscope analyses were performed on metal contacts and resist vias with no evidence of the interface damage or metal smearing commonly observed with mechanical polishing. Ion milling of the sample ex situ to the substrate provided decoration and adjustment of the exposed plane of the section when necessary for SEM analysis.     

Synthesis of PS and PDMAEMA mixed polymer brushes on the surface of layered silicate and their application in pickering suspension polymerization

An ammonium free radical initiator was ion exchanged onto the surface of clay layers. Polystyrene (PS) and poly(2‐(dimethylamino)ethyl methacrylate) (PDMAEMA) mixed polymer brushes on the surface of clay layers were prepared by in situ free radical polymerization. PS colloid particles armored by clay layers with mixed polymer brushes were prepared by Pickering suspension polymerization. Transmission electron microscopy (TEM), atomic force microscopy (AFM), and scanning electron microscopy (SEM) were used to characterize the structure and morphology of the colloid particles. Clay layers on the surface of PS colloid particles can be observed. Because of the cationic nature of the PDMAEMA brushes the colloid particles have positive zeta potentials at low pH values. X‐ray photoelectron spectroscopy (XPS) was used to analyze the surface of the colloid particles. N_1s binding energy of PDMAEMA chains on the surface of clay layers was detected by XPS. The two peaks of the N_1s binding energy indicate two different nitrogen environments on the surface of clay layers. The peak with a lower binding energy is characteristic of neutral nitrogen on PDMAEMA chains, and the peak with a higher binding energy is attributed to protonated nitrogen on PDMAEMA chains. © 2007 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 45: 5759–5769, 2007     

Characterization of etched glass surfaces by wave scattering

The roughness of glass surfaces after different stages of etching is investigated by reflection measurements with a spectrophotometer, light scattering, atomic force microscopy (AFM, on a small scale) and profilometry (on a large scale). The results suggest that there are three regimes during etching, according to their optical reflectivity and roughness. The first and the second regimes are studied by the Kirchhoff theory and the third one is studied by the optical geometric theory. Also, the roughness obtained by optical scattering is compared with the AFM results. Copyright © 2005 John Wiley & Sons, Ltd.     

Sol-Gel Route to Direct Formation of Silica Aerogel Microparticles Using Supercritical Solvents

A simple and versatile method to obtain silica aerogel particles based on the hydrolysis and subsequent condensation of silicon alkoxides in supercritical fluids is proposed. This microparticle production route reduces the number of steps of traditional microparticle sol-gel processing.A case example is explained in more detail. Spherical and fiber silica morphologies were obtained by a one step method using a sol-gel process with supercritical acetone as a solvent. Particle size was controlled by varying the relative amounts of alkoxysilane, water and acetone. The resulting materials are influenced by a large number of experimental parameters; it has been observed that a quite relevant one is the supercritical fluid venting rate. The morphology of the particles was characterized by electron microscopy (SEM and TEM) and Atomic Force Microscopy (AFM). Alternatively, a low temperature synthesis can be performed by using supercritical carbon dioxide as solvent and formic acid as condensation agent.