Comparative study of a block copolymer morphology by transmission electron microscopy and scanning force microscopy

Using transmission electron microscopy (TEM) and scanning force microscopy (SFM) together, it was possible to verify important structural features of a nanostructured bulk material such as the kp‐morphology in an ABC triblock copolymer. By applying suitable imaging techniques during the SFM measurements it was possible to determine the morphology without additional manipulation steps in between. In comparison, TEM investigations on this type of material usually require selective staining procedures prior to the measurement. Also electron beam damage is often encountered during TEM measurements especially if components such as poly(methacrylates) are present. In contrast, SFM measurements can be assumed not to significantly change the phase dimensions of the components.     

Low-voltage electron microscopy of polymer and organic molecular thin films

We have demonstrated the capabilities of a novel low-voltage electron microscope (LVEM) for imaging polymer and organic molecular thin films. The LVEM can operate in transmission electron microscopy, scanning transmission electron microscopy, scanning electron microscopy, and electron diffraction modes. The microscope operates at a nominal accelerating voltage of 5 kV and fits on a tabletop. A detailed discussion of the electron-sample interaction processes is presented, and the mean free path for total electron scattering was calculated to be 15 nm for organic samples at 5 kV. The total end point dose for the destruction of crystallinity at 5 kV was estimated at 5 x 10(-4) and 3.5 x 10(-2) C/cm2 for polyethylene and pentacene, respectively. These values are significantly lower than those measured at voltages greater than 100 kV. A defocus series of colloidal gold particles allowed us to estimate the experimental contrast transfer function of the microscope. Images taken of several organic materials have shown high contrast for low atomic number elements and a resolution of 2.5 nm. The materials studied here include thin films of the organic semiconductor pentacene, triblock copolymer films, single-molecule dendrimers, electrospun polymer fibers and gold nanoparticles.     

Tribological Behavior of Polyamide 66-Based Binary and Ternary Nanocomposites

The tribological behavior of polyamide 66 (PA66) and its composites filled with styrene?Cethylene/butylene?Cstyrene triblock copolymers (SEBS-g-MA) and organoclay nanolayers, were comprehensively investigated. Sliding tests were performed on a block-on-ring apparatus. We observed that the addition of the single organoclay filler leads to a decrease in the wear resistance of PA66. When SEBS-g-MA copolymers and organoclay nanolayers were added simultaneously to PA66, the wear resistance of PA66 improved remarkably. The corresponding morphologies of the worn surfaces further confirm this result. Differential scanning calorimetry measurements were also performed to observe the effect of fillers on the glass transition temperature (T _g). The T _g of the composites increased with the addition of organoclay and decreased with the addition of the SEBS-g-MA copolymers. The dispersion states of the SEBS-g-A copolymers and organoclay nanolayers in the PA66 matrix were examined by X-ray diffraction and transmission electron microscopy. The results indicate that the organoclay platelets and the SEBS-g-MA particles were well dispersed in the PA66 matrix.     

Histochemical demonstration of two subtypes of O-linked oligosaccharides in the rat gastric glands

The gastric glands synthesize glycoproteins whose oligosaccharides are linked to the peptide core mainly by the O-glycosidic bond, specifically removed by beta-elimination procedure. Our aim was to research the possibility of the existence of two subtypes of O-linked oligosaccharides with a different behavior to the removal procedure. The lectins from peanut (PNA) and Maackia amurensis (MAA-I) were histochemically used as markers of the O-linked oligosaccharides. Sections were also pretreated with beta-elimination and/or peptide N-Glycosidase F (PNGase-F) for the specific removal of O- and N-linked oligosaccharides, respectively. The lectin GNA, which mainly labels to N-linked oligosaccharides, was used to test the correct working of PNGase-F. To test the possibility that the beta-elimination treatment could remove the terminal sialic acid residues, the lectin LFA was used. The surface epithelium was negative to PNA, while it became strongly positive when beta-elimination was performed for 1 day. This staining was resistant to PNGase-F, suggesting that PNA was labeling to O-linked oligosaccharides. However, after beta-elimination for 5 days this staining is not observed. A similar pattern appeared with MAA-I. We propose the existence of two subtypes of O-linked oligosaccharides: labile and resistant. The labile O-linked oligosaccharides are removed with beta-elimination for 1 day, unmasking the PNA-positive oligosaccharides. These oligosaccharides are resistant O-linked oligosaccharides because staining is abolished with longer treatment of beta-elimination. The results with MAA-I also support this suggestion. In summary, the labile O-linked oligosaccharides are removed with short treatment, while the resistant O-linked oligosaccharides need a stronger procedure (for 5 days).     

SEM-EDS technique employed in evaluating the aggregation behaviors of amphiphilic ABC-type triblock copolymers in mixed solvents with tuned polarities

In this paper, a scanning electron microscopy‐energy dispersive spectroscopy (SEM‐EDS) technique has been developed for evaluating the aggregation structure of amphiphilic fluorinated ABC‐type triblock copolymers MeOPEO₁₆‐PSt₂₂₀‐PFHEA₂₂ in mixed solvents with different polarities. The polarities of mixed solvents can be tuned by changing volume ratios of toluene, anhydrous ethanol, and distilled water, which leads to the changes in morphology and size of self‐assembled colloidal particles of the copolymers in the system. The aggregation behaviors of the copolymers are revealed by SEM, transmission electron microscopy (TEM), and corresponding SEM‐EDS techniques. The variations in concentrations of O and F elements over the thickness of copolymers particles give direct evidence for a better understanding of the arrangement of each block segment of copolymers in solution. And the technique can also help to explain the aggregation structure of micro‐ or nanomaterial with shell‐core structure. Microsc. Res. Tech., 2011. © 2011 Wiley Periodicals, Inc.     

Herpes simplex virus-mediated expression of the axonal protein tau in human model neurons (NT2-N cells)

The establishment of axonal-somatodendritic polarity is an important event during neuronal development. The analysis of the underlying molecular events requires experimental models that display characteristic steps in the development of polarity and that are accessible for experimental manipulations. Here we show that human model neurons (NT2-N cells) can be efficiently infected with an amplicon-based herpes simplex virus (HSV) system that expresses the axonal microtubule-associated protein tau. We demonstrate that the neurons express a high level of exogenous tau, which persists for several days, thus allowing us to analyze the morphological effects of the expressed protein. The intracellular interactions of tau and the effects on the microtubule structure of infected neurons, which were processed for immunocytochemistry, were determined using laser scanning microscopy (LSM). Exogenous tau expression does not result in an increased axon growth of the neurons but promotes neuronal microtubule assembly as indicated by an increased amount of total microtubule polymer as well as a labile, detyrosinated microtubule subpopulation. In contrast, tau expression does not induce a significant microtubule stabilization as judged from the quantitation of acetylated microtubule staining 24 hours after infection. The data demonstrate that HSV-mediated expression of proteins in human model neurons provides a useful system for analysis of the effect of neuronal proteins on the morphology and cytoskeletal organization of terminally differentiated polar neurons. In addition, it suggests a role for tau as a factor which locally promotes tubulin polymerization while the dynamics of axonal microtubules are preserved.     

全息方法制备嵌段式液晶弹性体

研究了热致收缩形变三嵌段式液晶(LC)弹性体薄膜的制备方法,分析和测试了薄膜的偏光特性和热致收缩率.采用全息曝光的方法一次性制备出具有栅状结构的热致液晶弹性体薄膜材料.在此基础上采用偏光显微镜(POM)、He-Ne激光器对弹性体薄膜的嵌段式栅状结构和偏光特性进行检测,并分析了薄膜弹性体偏光特性和液晶分子取向的关系,对该...     

Adsorption structure and adhesion strength of aqueous copolymer lubricant films on Si surface

The adsorption structure of aqueous triblock copolymer polypropylene oxide‐polyethylene oxide‐polypropylene oxide, PPO‐PEO‐PPO, on the Si surface was studied using neutron reflectometer. It is found that PEO blocks formed the outer layer of the adsorbed PPO‐PEO‐PPO film, while PPO blocks formed the inner layer and served as the anchor blocks. The adhesion strength of adsorbed PPO‐PEO‐PPO copolymer film was evaluated using atomic force microscopy and scratch tests. The results revealed that the molecular structure of triblock copolymer had a considerable effect on the adhesion strength. The triblock copolymer with a longer PPO chain and a higher weight percentage of PPO exhibited stronger adhesion and better lubrication performance.     

高分辨快原子轰击质谱分析核苷类似物

本文应用高分辨快原子轰击质谱 ( HRFAB- MS)分析了 6个含有二个糖的核苷类似物 ,测定了它们分子离子和特征离子的精确分子量 ,并确定了其分子式。     

In situ synthesis of carbon nanotubes on heated scanning probes using dip pen techniques

Carbon nanotubes (CNT) were synthesized on heated scanning probes and under ambient conditions without requiring Chemical vapor deposition (CVD) apparatus or process gases. In this study, dip pen nanolithography (DPN) techniques were utilized for deposition of catalyst precursors on the scanning probe tips in the form of aqueous solution of metal salts--prior to the synthesis of the CNT. A layer of fullerene (C(60)) of approximately 200 nm thickness was vapor deposited on the scanning probe tip prior to the deposition of the metal catalyst. During the in situ synthesis of the CNT on the scanning probes, the temperature of the heated scanning probes reached 350-400 degrees C. Hence the scanning probes were heated in an inert atmosphere to prevent potential oxidation of the deposited fullerene layer. The synthesized CNTs were subsequently characterized using SEM and Raman spectroscopy. The Raman spectroscopy showed peaks in the Radial breathing mode (RBM), as well as the defect (D) and graphitic (G) bands. The RBM peaks indicate that the single walled carbon nanotube (SWCNT) ranged in diameter from 0.9-1.5 nm. The peaks in the Raman spectra are indicative of SWCNT mixtures (metallic and semconducting) and possibly multiwalled carbon nanotube (MWCNT). Hence this process can be optimized to synthesize SWCNT of a specific chirality (metallic or semiconducting). This study differs from an earlier study reported in the literature involving synthesis of CNT on scanning probes where the process temperatures typically exceeded 700 degrees C, and resulted in synthesis of highly graphitic MWCNT (Sunden, et al., 2006).     

Phase Behavior and Lubricity of Aqueous PEO-PPO-PEO and PPO-PEO-PPO Triblock Copolymer Solutions

Aqueous triblock copolymer solutions are potential low-cost, eco-friendly lubricants. However, as a solution, their phase changes with copolymer concentration and solution temperature, raising the question, “Does the phase change affect the formation of adsorbed layer and the lubrication performance?” This article studies the copolymer solution phase behavior and lubricity in response to the copolymer structure, concentration, and solution temperature. Four different triblock copolymers, two normal PEO-PPO-PEO and two reverse PPO-PEO-PPO composed of PEO poly(ethylene oxide) and PPO poly(propylene oxide), have been investigated. From cloud point and surface tension measurements, phase change and micellization are shown to depend on copolymer type, number of hydrophilic PEO blocks, and temperature. Furthermore it is found that the phase and the presence of micelles lead to significant variation in adsorbed copolymer mass and lubricity. Based on the observed phase behaviors, the lubricity of copolymer solutions is discussed with regard to aggregation and adsorption on the solid–liquid interface.     

Characterization of a diesel sludge microbial consortia for bioremediation

The organisms found growing in a mixed diesel sludge-chromium metal waste were characterized directly using environmental scanning electron microscopy (ESEM) and traditional fixation techniques with scanning electron microscopy (SEM). An attempt to identify organisms genetically directly from the sludge failed because of interference from chemicals in the waste with polymerase chain reaction (PCR). The organisms were isolated using plate culture techniques and isolates were characterized by SEM and genetic sequencing. A variety of organisms were found with differing morphologies and growth habits. Sequencing identified an organism homologous to Bacillus mycoides and matched other organisms such as Paenibacillus lautus, Paenibacillus spp., Bacillus spp., and Rhodobacter spp.     

Cold-spray Ionization Mass Spectrometry for Characterization of Biomolecules in Solution

A direct solution analysis method, coldspray ionization (CSI) mass spectrometry (MS)[1], a variant of electrospray (ESI) MS operating at low temperature (ca. - 80 ～ 10℃), allows facile and precise characterization of labile organic species, especially those in which non-covalent bonding interactions are prominent. We have applies this method to investigations of the solution structures of many labile organic species, including unstable reagents and reaction intermediates, asymmetric catalysts, supramolecules, and even primary biomolecules.     

Polyethylene glycol (PEG) embedding and subsequent de-embedding as a method for the correlation of light microscopy,scanning electron microscopy,and transmission electron microscopy

The polyethylene glycol (PEG) embedding and subsequent deembedding method was applied to the observation of general tissues in scanning electron microscopy (SEM). Resulting SEM images were of high quality. It was demonstrated that intermicroscopic correlation of images between light microscopy (LM), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) is easily and reliably done by means of the PEG method. In particular, the exact correlation of immuno-LM with SEM is shown to be of potential value.     

Shear force imaging of DNA in a near-field scanning optical microscope (NSOM)

A near-field scanning optical module has been constructed as an accessory for a Nanoscope IIIa commercial scanning probe microscope. Distance feedback and topographic registration are accomplished with an uncoated optical fibre scanning tip by implementation of the shear force technique. The tip is driven by a piezoelectric actuator at a resonance frequency of 8–80 kHz. A laser diode beam is scattered by the tip and detected by a split photodiode, with lock-in detection of the difference signal. The amplitude ( r ) and phase (τ) responses were characterized as a function of the calibrated tip–sample separation. Using an r cos τ feedback signal, imaging of pUC18 relaxed circular plasmid DNA spread on mica precoated with cetylpyridinium chloride was achieved. The apparent width (28 ± 5 nm) was approximately four times that achieved by scanning force measurements with the same instrument; the apparent height of the DNA (0.6 ± 0.3 nm) was similar with the two techniques. These results demonstrate the applicability of the shear force signal for imaging biological macromolecules according to topography and in conjunction with the optical signals of a near-field scanning optical microscope (NSOM).     

Ti_3SiC_2材料的力学性能及抗损伤机制

利用反应烧结技术得到了纯度为93.0%的Ti3SiC2块体材料;测试了该材料的断裂强度和硬度;用XRD、SEM等方法分析了材料的物相组成、断口形貌和损伤机制;用TG/DTA法分析了气孔产生的原因.结果表明:1 250℃烧结Ti3SiC2材料的抗弯强度为105.59 MPa,硬度为101 HB;其强度随Ti3SiC2含量的增加而增大;材料的抗损伤机制是通过晶粒破碎、穿晶断裂、分层、拔出等形式来消耗能量,从而阻止了裂纹的扩展,表现出了一定的微塑性.     

双（氢化牛脂基）二甲基季铵化合物的质谱裂解规律及色谱分离研究

建立了高效液相色谱-电喷雾串联质谱（HPLC-ESI-MS/MS）联用技术快速鉴定和检测双（氢化牛脂基）二甲基季铵化合物（DHTDMAC）的方法。通过对双（氢化牛脂基）二甲基氯化铵标准品的质谱解析,由一级质谱中各成分的特征母离子峰和二级质谱裂解碎片,得出质谱裂解规律,并推断出标准品中所包含的16种DHTDMAC组分。通过中性丢失扫描、母离子扫描和子离子扫描对质谱解析和裂解规律进行了验证。通过色谱条件的优化,采用电喷雾电离正离子（ESI⁺）、多反应监测（MRM）模式,建立了色谱分离、质谱检测的方法。本研究鉴定出不同链长烷基和碳数的DHTDMAC组分,并建立了DHTDMAC单个组分的简便、高效的检测方法,对准确研究该类化合物,以及加强环境、化工产品和消费品中DHTDMAC的监控提供了依据。     

X-ray probe microanalyses and scanning x-ray microscopies

The analytical techniques based on excitation of inner-shell electrons by an incident X-ray photon beam suffer generally from their poor degree of lateral localization. Nevertheless it is possible to perform the microanalysis of a sample in the forms of a thin film by: (i) X-ray photoelectron spectroscopy (XPS or ESCA) and X-ray-induced Auger electron spectroscopy (XAES) for surface analysis; (ii) X-ray absorption spectroscopy (XAS) and X-ray microfluorescence spectroscopy (XMS) for bulk analysis. The corresponding images can also be obtained in the scanning mode: scanning X-ray photoelectron microscopy (SXPM), scanning X-ray-induced Auger electron microscopy (SXAEM) and scanning X-ray microradiography (SXM). The experimental arrangement and the results obtained are described here, together with further improvements and comparisons with other technical solutions.     

表面形态对铝合金表面注射结合性能的影响

通过对铝合金表面进行阳极氧化和偶联剂处理,提出了一种注塑工艺直接成形铝合金聚酰胺复合构件的方法。利用激光共焦扫描显微镜和傅里叶红外(FTIR)光谱仪对经处理过的铝合金表面结构和成分进行了分析,结果表明：铝合金表面粗糙度和偶联剂固化时形成的Si-O-Al、C-N等化学键对界面结合力有重要影响。讨论了阳极氧化工艺参数和偶联剂固化条件对铝合金表面形貌、成分和注塑复合构件力学性能的影响规律,借助扫描电子显微镜(SEM)分析了复合构件拉伸剪切的破坏机理。     

Spot counting to locate fetal cells in maternal blood and tissue: a comparison of manual and automated microscopy

BACKGROUND: Fetal cell detection in maternal tissue requires an accurate, efficient, and reproducible microscopy method. Our objective was to compare manual scoring to a commercially available automated scanning system for the detection of chromosome signals by fluorescence in situ hybridization (FISH). METHODS: X and Y chromosome FISH signals were detected on slides of calibrated mixtures of blood, paraffin-embedded liver sections, and post-termination blood. For manual scoring (400x magnification), the number of cells located and duration of scoring were recorded. For automated scanning using the Metasystems Metafer3/Metafer4 Scanning System (200x magnification), duration of scanning, number of gallery images generated, duration of manual review of gallery images, and number of confirmed fetal cells were recorded. RESULTS: From all slides the number of target fetal cells located by manual and automated microscopy was highly correlated (r = 0.90). However, automated scanning required on average 4-fold more time than manual scoring (P < 0.0001), with an average automated scanning time of 9.7 h per slide compared with 2.4 h per slide when scored manually. CONCLUSIONS: In general, the accuracy of automated and manual microscopy is comparable, although manual scoring is more efficient because of the level of magnification necessary for automated scanning of cells, and a large number of gallery images generated by automated scanning that must then be reviewed manually. This suggests that when rapid analysis is required (i.e., clinical situations), manual microscopy is preferable. In contrast, automated scanning may have advantages over manual microscopy when time constraints are less imposed (i.e., research situations).