环境扫描电子显微镜的特性及应用概况

简要叙述了环境扫描电子显微镜的原理,着重介绍了它的特性和在国内外应用的概况。与普通的扫描电子显微镜相比,它具有能直接检测不导电样品和含油含水样品的独特性能,为扫描电子显微镜的应用开拓了新的领域。     

Characterisation and intrinsic magnetic resonance properties of nickel nanoparticles

Nickel nanoparticles have been extensively characterised by atomic force microscopy (AFM), scanning electron microscopy (SEM) and confocal micro-Raman spectroscopy. AFM underestimates the particle size compared to SEM measurements. It is shown that Raman spectroscopy can detect the nanometre-thick NiO layer on the particles having frequency shifts of the modes indicative of phonon confinement. The magnetic properties of the particles are studied by ferromagnetic resonance (FMR) of magnetic field aligned particles. The alignment is achieved by suspending the particles in the liquid crystal MBBA and freezing the liquid in a 0.4 T DC magnetic field. The in-field solidification locks the direction of maximum magnetisation of the particles parallel to the direction of the applied DC magnetic field. This removes the effects of dynamical particle fluctuations of the nanoparticles on the magnetic properties allowing a study of the intrinsic magnetic properties of the magnetic nanoparticles. The intensity of the FMR signal decreased with lowering temperature for the particles frozen in the liquid in a 0.4 T DC magnetic field. The effect is suggested to be due to a reduction of the microwave skin depth with lowering temperature.     

催化裂解聚苯乙烯制备碳纳米管的研究

通过在60℃氮气气氛中催化裂解聚苯乙烯,制备了大量管径为5～40nm的高质量的碳纳米管.利用扫描电子显微镜、透射电子显微镜和拉曼光谱对所制备的碳纳米管进行了表征.研究表明,所制备的碳纳米管石墨化程度高,在碳纳米管的管壁上仅有少量的无定形碳存在.催化裂解聚苯乙烯制备碳纳米管是一种有前途、低成本的绿色化学方法.     

Transdermal delivery of car vedilol in rats: probing the percutaneous permeation enhancement mechanism of soybean extract–chitosan mixture

Background: This study was designed for investigating the effect of soybean (SS) extract and chitosan (CTN) in facilitating the permeation of carvedilol (CDL) across rat epidermis. Method: Transdermal flux of carvedilol through heat-separated rat epidermis was investigated in vitro using vertical Keshary–Chien diffusion cells. Biophysical and microscopic manifestations of epidermis treated with SS-extract, CTN, and SS extract–CTN mixture were investigated by using DSC, TEWL, SEM, and TEM. Biochemical estimations of cholesterol, sphingosine, and triglycerides were carried out for treated excised as well as viable rat epidermis. The antihypertensive activity of the patches in comparison to that after oral administration of carvedilol was studied in deoxycorticosterone acetate-induced hypertensive rats. Results: The solubility of CDL was found to be maximum in the presence of 1% (w/v) SS extract. The K_IPM/PB of CDL decreased with increase in concentration of SS extract. The in vitro permeation of CDL across rat epidermis increased and was maximum with combination of SS extract and chitosan (CTN). Biochemical and microscopic studies revealed the initiation of reversal of barrier integrity after 12 hours. Furthermore, the application of patches containing SS extract–CTN mixture resulted in sustained release of carvedilol, which was able to control the hypertension in deoxycorticosterone acetate (DOCA) induced hypertensive rats through 24 hours. CTN was found to potentiate the permeation enhancing activity of SS extract. Conclusion: The developed transdermal patches of CDL containing SS extract–CTN mixture exhibited better performance as compared to oral administration in controlling hypertension in rats.     

Phase Identification in a Scanning Electron Microscope Using Backscattered Electron Kikuchi Patterns

Backscattered electron Kikuchi patterns (BEKP) suitable for crystallographic phase analysis can be collected in the scanning electron microscope (SEM) with a newly developed charge coupled device (CCD) based detector. Crystallographic phase identification using BEKP in the SEM is unique in that it permits high magnification images and BEKPs to be collected from a bulk specimen. The combination of scanning electron microscope (SEM) imaging, BEKP, and energy dispersive x-ray spectrometry holds the promise of a powerful new tool for materials science.     

扫描电镜中荷电效应的分析

扫描电子显微镜要得到层次清晰、立体感强且分辨率高的高质量图像,荷电效应是一个重要的影响因素。对在扫描电子显微镜成像中荷电效应的成因及其解决办法进行了系统的分析。提出采用镀膜、降低加速电压及低真空的方法,可降低荷电效应的影响。     

有关电子显微技术的几个实验和建议

本文涉及两个和电子显微技术有关的问题：豆．透射电子显微镜试样薄片表面沉淀相颗粒存在状况的实验观察．２．扫描电子显微镜背反射电子象用作定量金相测定的建议。     

Calibration of High-Resolution X-Ray Tomography With Atomic Force Microscopy

For two-dimensional x-ray imaging of thin films, the technique of scanning transmission x-ray microscopy (STXM) has achieved images with feature sizes as small as 40 nm in recent years. However, calibration of three-dimensional tomographic images that are produced with STXM data at this scale has not yet been described in the scientific literature, and the calibration procedure has novel problems that have not been encountered by x-ray tomography carried out at a larger scale. In x-ray microtomography, for example, one always has the option of using optical imaging on a section of the object to verify the x-ray projection measurements; with STXM, on the other hand, the sample features are too small to be resolved by light at optical wavelengths. This fact implies that one must rely on procedures with higher resolution, such as atomic force microscopy (AFM), for the calibration. Such procedures, however, generally depend on a highly destructive sectioning of the sample, and are difficult to interpret because they give surface information rather than depth information. In this article, a procedure for calibration is described that overcomes these limitations and achieves a calibration of an STXM tomography image with an AFM image and a scanning electron microscopy image of the same object.A Ge star-shaped pattern was imaged at a synchrotron with a scanning transmission x-ray microscope. Nineteen high-resolution projection images of 200 × 200 pixels were tomographically reconstructed into a three-dimensional image. Features in two-dimensional images as small as 40 nm and features as small as 80 nm in the three-dimensional reconstruction were resolved. Transverse length scales based on atomic force microscopy, scanning electron microscopy, x-ray transmission and tomographic reconstruction agreed to within 10 nm. Toward the center of the sample, the pattern thickness calculated from projection images was (51 ± 15) nm vs (80 ± 52) nm for tomographic reconstruction, where the uncertainties are evaluated at the level of two standard deviations.     

电子显微分析技术在奥氏体合金应力腐蚀开裂研究领域中的应用

奥氏体合金广泛应用于核电领域。应力腐蚀开裂是核电材料主要的失效形式之一,奥氏体合金的应力腐蚀开裂关系到核电站的安全运行。综述了评估应力腐蚀开裂的试样方法以及运用现代电子显微分析技术表征应力腐蚀开裂的方法。对这些电子显微分析技术的优点进行了总结,并指出未来电子显微分析技术在应力腐蚀开裂研究中的发展方向。     

Optical Emission Study of RF Thermal Plasma During Fullerene Synthesis

Results on studies of molecular spectra emitted in the initial stages of fullerene synthesis during processing of graphite powder in RF thermal plasma conditions are presented in this work. CN—usually present in carbon plasmas—and C₂ were found as dominant molecular species. The role of CN radicals on the fullerene formation was discussed in detail. Intensities of CN and C₂ lines were studied against the composition of gas phase and the feed rate of graphite powder. The rotational-vibrational temperatures of CN species were calculated by fitting the experimental spectra to the simulated ones. It was concluded that in the plasma region CN radicals could be formed by the reaction of C₂ with atomic nitrogen at smaller loads. This reaction lowered the yield of fullerenes. At larger loads, C₂ formation was decreased due to lower temperature of the particles compared to smaller load. The CN radicals were produced by the surface reaction of the hot carbon particles with nitrogen atoms. Results confirmed that for effective fullerene synthesis, the nitrogen content of the precursors and the plasma gases should be minimized.     

Crystalline and amorphous carvedilol-loaded nanoemulsions: formulation optimisation using response surface methodology

This study aimed to evaluate the crystalline and amorphous carvedilol along with their lipidic mixtures using various instrumental techniques and to use response surface methodology in conjunction with factorial design to establish the functional relationships between operating variables (capmul GMS 50?K and cremophor RH 40).

The response variables selected are spectroscopic absorbance (Y ₁), mean particle size in distilled water (Y ₂) and in phosphate buffer pH 6.8 (Y ₃), polydispersibility index (PDI) (Y ₄) and zeta potential (Y ₅).

The optimal formulations of crystalline and amorphous carvedilol-loaded nanoemulsions were composed of fixed levels, ?0.41 and ?0.42, of capmul GMS 50?K and cremophor RH 40, respectively. The predicted and observed values of Y ₁–Y ₅ for blank nanoemulsions showed the percentage bias error of ?12.12%, ?10.25%, ?18.47%, +14.81 and ?2.89, respectively. The bias percent ranged between ?2.70% and ?29.41% for the responses Y ₁–Y ₄ for both crystalline and amorphous carvedilol-loaded nanoemulsions, indicating high degree of prognosis. However, the bias percent values for the response variable Y ₅ were 294.2% and 262.6%, for the crystalline and amorphous carvedilol-loaded nanoemulsions, respectively, possibly due to cationisation of emulsion droplets. The transmission electron microscopy of selected optimal nanoemulsions showed the spherical shape of globules with no signs of coalescence and precipitation of drug.

This study demonstrates the use of factorial design for the preparation of nanoemulsions of crystalline and amorphous carvedilol. The desirable goals can be obtained by systematic formulation approach in the shortest possible time.     

二极溅射沉积Fe-N-O薄膜的形貌与结构分析

利用二极溅射的方法在不同衬底上沉积了Fe N O薄膜。通过扫描电子显微镜(SEM)、光电子能谱(XPS)和透射电子显微镜(TEM)等先进实验分析手段对二极溅射沉积Fe N O薄膜的形貌与结构进行了分析。XPS和TEM的结果表明,薄膜的主要成分为FeO和少量的Fe16N2多晶体组成,生长上存在择优取向;表面均匀、致密、平整,晶粒大小在50nm左右。     

Nanohydroxyapatite shape and its potential role in bone formation: an analytical study

Bone cells (osteoblasts) produce a collagen-rich matrix called osteoid, which is mineralized extracellularly by nanosized calcium phosphate (CaP). Synthetically produced CaP nanoparticles (NPs) have great potential for clinical application. However few studies have compared the effect of CaP NPs with different properties, such as shape and aspect ratio, on the survival and behaviour of active bone-producing cells, such as primary human osteoblasts (HOBs). This study aimed to investigate the biocompatibility and ultrastructural effects of two differently shaped hydroxyapatite [Ca₁₀(PO₄)₆(OH)₂] nanoparticles (HA NPs), round- (aspect ratio 2.12, AR2) and rice-shaped (aspect ratio 3.79, AR4). The ultrastructural response and initial extracellular matrix (ECM) formation of HOBs to HA NPs were observed, as well as matrix vesicle release. A transmission electron microscopy (TEM)-based X-ray microanalytical technique was used to measure cytoplasmic ion levels, including calcium (Ca), phosphorus (P), sodium (Na) and potassium (K). K/Na ratios were used as a measure of cell viability. Following HA NP stimulation, all measured cytoplasmic ion levels increased. AR2 NPs had a greater osteogenic effect on osteoblasts compared with AR4 NPs, including alkaline phosphatase activity and matrix vesicle release. However, they produced only a moderate increase in intracellular Ca and P levels compared with AR4. This suggests that particular Ca and P concentrations may be required for, or indicative of, optimal osteoblast activity. Cell viability, as measured by Na and K microanalysis, was best maintained in AR2. Initial formation of osteoblast ECM was altered in the presence of either HA NP, and immuno-TEM identified fibronectin and matrilin-3 as two ECM proteins affected. Matrilin-3 is here described for the first time as being expressed by cultured osteoblasts. In summary, this novel and in-depth study has demonstrated that HA NP shape can influence a range of different parameters related to osteoblast viability and activity.     

Determination of the composition of binary systems by the ratio method employing SEM-EDAX

By employing x-ray emission in a scanning electron microscope (SEM), it has been shown that compositions of binary systems such as As-Se glasses, Al-Zn alloys and copper sulphides can be determined.     

Effect of acetylene flow rate on morphology and structure of carbon nanotube thick films grown by thermal chemical vapor deposition

Carbon nanotube (CNT) films were grown on nickel foil substrates by thermal chemical vapor deposition (CVD) with acetylene and hydrogen as the precursors. The morphology and structure of CNTs depending on the acetylene flow rate were characterized by a scanning electron microscope (SEM), a transmission electron microscope (TEM) and a Raman spectrometer, respectively. The effect of acetylene flow rate on the morphology and structure of CNT films was investigated. By increasing the acetylene flow rate from 10 to 90 sccm (standard cubic centimeter per minute), the yield and the diameter of CNTs increase. Also, the defects and amorphous phase in CNT films increase with increasing acetylene flow rate. Translated from Journal of Inorganic Materials, 2006, 21(1): 75–80 [译自: 无机材料学报]