Analysis of thermal effects accompanying the interaction of electron beams with ferroelectric crystals

A spatial nonstationary temperature distribution in a model ferroelectric specimen exposed to electron beams of a scanning electron microscope (SEM) is simulated. A solution to the problem on the effect of focused heat sources having different configurations on a single ferroelectric crystal and crystal with electrodes deposited on its faces is presented. The model is based on the finite-difference method. A program for calculating temperature fields and maximum overheating temperature for preset specimen characteristics and experimental parameters of different scanning electron microscopes is suggested.     

Secondary-electron SEM bioimaging of human erythrocytes in bloodstains on high-carbon steel substrate without specimen preparation

The imaging of most biological samples via conventional scanning electron microscope (SEM) in secondary-electron mode involves routinely some kind of specimen preparation. Conventional SEMs are still used when a low-vacuum or variable-pressure SEM (usually known as 'environmental', or ESEM) is not available. But that preparatory approach may be undesirable in certain cases, for instance in museum specimens, forensic evidences or clinical samples. This report details a simple, low-cost, and sample-saving bioimaging protocol without specimen preparation, by using removable plastic conducting carbon cement, and then working under ex-profeso SEM conditions, i.e., by using an SEM in secondary-electron mode just like an ESEM. The successful use to image up to high magnifications human erythrocytes in bloodstains on an extensively bloodsmeared, high-carbon steel surgical blade is reported as an example of the potential of this procedure.     

Aligned synthesis of multi-walled carbon nanotubes with high purity by aerosol assisted chemical vapor deposition: Effect of water vapor

Aligned multi-walled carbon nanotubes (MWCNTs) with high purity and bulk yield were achieved on a silicon substrate by an aerosol-assisted chemical vapor deposition. The introduction of specific amounts of water vapor played a key role in in situ controlling the purity and surface defects of the nanotubes. The morphology, surface quality and structure of MWCNTs were characterized by secondary and backscattered electron imaging in a field emission scanning electron microscope (FESEM) and transmission electron microscope (TEM). Crystallinity and defects of the MWCNTs’ were investigated by high-resolution transmission electron microscopy (HRTEM) and Raman spectroscopy. In this work, water vapor was found to provide a weak oxidative environment, which enhanced and purified the MWCNTs’ growth. However, excessive water vapor would inhibit the MWCNTs growth with a poor surface quality. In addition, it has been found that the surface morphology of the CNTs can be modified intentionally through producing some surface defects by tuning the amount of the water vapor, which may offer more nucleation sites on the chemically inert CNT surface for various applications such as catalyst support.     

Observations of the intestinal mucosa using environmental scanning electron microscopy (ESEM); comparison with conventional scanning electron microscopy (CSEM)

In order to evaluate the potential use of environmental scanning electron microscopy (ESEM) in biology, structural changes of the jejunal villi of rats were studied after periods of fasting and refeeding, using a conventional scanning electron microscope (CSEM) and ESEM. While observation using the CSEM, involves chemical fixation, drying and coating, observation of fresh, unprepared materials can be directly realized with the ESEM. Environmental microscopy provides a relatively new technology for imaging hydrated materials without specimen preparation and conductive coating. Direct observation of biological samples in their native state is therefore possible with an ESEM.

After fasting, the jejunal mucosa is dramatically reduced in size, splits and holes appearing at the tip of the villi. These changes were observed whatever the type of technique used. Artifacts due to the sample preparation for CSEM observation (drying, coating) can therefore be excluded. However, CSEM and ESEM must be used jointly. While, CSEM must be preferred for surface analysis involving high magnifications, ESEM observation, on the other hand, can prove valuable for determining the living aspect of the samples.     

SEM imaging of liquid jets

We present a technique for the study of liquid jets in an environmental scanning electron microscope (ESEM). By using a two-fluid stream consisting of a water inner core and a co-flowing outer gas sheath, we are able to produce liquid streams of sufficiently low flow rate to be compatible with ESEM vacuum requirements. We have recorded ESEM images of water jets down to 700 nm diameter. Details of the jet structure, such as the point of jet breakup and size and shape of the jet cone, can be measured with ESEM to far greater accuracy than with optical microscopy. ESEM imaging of liquid jets offers a valuable research tool for the study of aerosol production, combustion processes, ink-jet generation, and many other attributes of micro- and nanojet systems.     

Microstructure and microhardness analysis of the hexagonal oxides formed on the surface of the AISI 304 stainless steel after Nd:YAG pulsed laser surface melting

The laser surface melting (LSM) technique was adopted to modify the surface layer microstructure of the AISI 304 stainless steel in this paper. The results showed that the hexagonal morphologies have been successfully fabricated on the surface after LSM. These hexagons had side lengths of about 0.5-1 μm and were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), field emission scanning electron microscope (FESEM) and high resolution transmission electron microscope (HRTEM). It was proved by the XRD that the stainless steel surface mainly consisted of γ-Fe, Cr₂O₃, Fe₂O₃ and some manganese oxides. The FESEM micrographs showed that the hexagonal oxides were regular hexagons in geometry. The HRTEM micrographs also indicated the presence of the hexagons on the surface of the stainless steel. The spacing values were calculated from the HRTEM micrograph and the SAED pattern, and the hexagonal oxide phases determined by these spacing values were consistent with those verified by the XRD. After LSM, the microhardness of the stainless steel was significantly improved.     

Characterization of martensite in Fe-25%Ni-15%Co-5%Mo alloy

Kinetic, morphological, crystallographical, magnetic and thermal characteristics of thermally induced martensite in Fe-25%Ni-15%Co-5%Mo alloy have been investigated by scanning electron microscope (SEM), transmission electron microscope (TEM), Mössbauer spectrometer, and differential scanning calorimeter (DSC). Kinetics of the transformation was found to be athermal. Also only lenticular martensite morphology was observed during microscope observations. In addition, martensite start temperature (M_s) was determined as −63 °C from differential scanning calorimeter. On the other hand, Mössbauer spectra revealed a paramagnetic character for the austenite phase and a ferromagnetic character for thermally induced martensite phase.     

Microscopic analysis of surface state of SUS-304L stainless steel by low energy scanning electron microscopy in ultra high vacuum

The variation of surface state of SUS-304L stainless steel with heat treatment in a vacuum of 10^?9 Torr was observed by the ultra high vacuum low energy scanning electron microscope (UHVLESEM) by detecting the absorption electron current. The absorption electron current was very sensitive to the surface state and a large effect of the electron beam irradiation was observed. The variation of the absorption electron current with the surface segregation was measured within a microscopical dimension of 0.3 microm on a selected area of the scanning electron microscopic image. At the same time, the surface state was characterized by Auger electron spectroscopy and relations between surface states and the absorption electron current were discussed in relation to the secondary electron and backscattered electron yields.     

Decoration of copper oxide nanoplatelets with gold nanoparticles by laser ablation in methanol for photodetection applications

In this work, CuO/n-Si and AuNPs-decorated CuO/n-Si heterojunction photodetectors were fabricated by deposition of CuO nanoplatelets and Au nanoparticles NPs decorated CuO nanoplatelets on silicon substrates by laser ablation in methanol. Atomic force microscope AFM, scanning electron microscope SEM and transmission electron microscope TEM were used to study the structural and surface morphology of CuO and AuNPs–CuO. The electrical properties showed that the CuO/Si and AuNPs decorated-CuO/Si showed rectifying behavior. The maximum values of quantum efficiency were about 41 and 78% at 700 nm for CuO/Si and AuNPs–CuO/Si photodetectors, respectively. The I–V characteristics of the photodetectors were measured under UV light.     

Electron microscopes using field emission source

The high brightness and small physical dimensions of a field emission source make it extremely attractive as the source of electrons in scanning electron microscopes. Using this kind of source considerable improvements have been made in this type of instrument so that at the present time the surfaces of solid objects can be viewed at a resolution of 30 Å and thin specimens can be viewed with a resolution of 2.5 Å. The particular nature of the scanning electron microscope allows some unique forms of contrast to be obtained so that the micrographs which can be taken with these microscopes are different in content and quality than those taken on conventional microscopes. As one example, we have been able to study the motion of single heavy atoms on thin carbon films. The resolution is, of course, not as high as that which can be obtained with a field ion microscope but the kind of specimen which can be viewed is different so that the two instruments are complementary in nature.     

Low voltage high-resolution SEM (LVHRSEM) for biological structural and molecular analysis

High-resolution scanning electron microscopy (HRSEM) is being used increasingly to gain new insights into three-dimensional organization of biological structure, macromolecular complexes and interactions of cellular components as well as isolated cell organelles. Modern scanning electron microscopes (SEMs) combined with adequate sample preparation can now provide resolution comparable with that achieved using transmission electron microscopes (TEMs) down to 2-5 nm for biological material. The versatility of the instrument and new sample preparation techniques have allowed detailed analysis of chromosomes, cytoskeletal components, virus and other biological material that has not been possible with TEM. The present review addresses resolution and specific specimen preparations for HRSEM, and highlights the importance of specimen preparation and choice of methods to achieve optimal results for proteins, macromolecular complexes and subcellular structures using low voltage HRSEM (LVHRSEM).     

Imaging of Norway spruce early somatic embryos with the ESEM,Cryo-SEM and laser scanning microscope

This article describes the surface structure of Norway spruce early somatic embryos (ESEs) as a typical culture with asynchronous development. The microstructure of extracellular matrix covering ESEs were observed using the environmental scanning electron microscope as a primary tool and using the scanning electron microscope with cryo attachment and laser electron microscope as a complementary tool allowing our results to be proven independently. The fresh samples were observed in conditions of the air environment of the environmental scanning electron microscope (ESEM) with the pressure from 550 Pa to 690 Pa and the low temperature of the sample from −18 °C to −22 °C. The samples were studied using two different types of detector to allow studying either the thin surface structure or material composition. The scanning electron microscope with cryo attachment was used for imaging frozen extracellular matrix microstructure with higher resolution. The combination of both electron microscopy methods was suitable for observation of “native” plant samples, allowing correct evaluation of our results, free of error and artifacts.     

A history of scanning electron microscopy developments: towards "wet-STEM" imaging

A recently developed imaging mode called "wet-STEM" and new developments in environmental scanning electron microscopy (ESEM) allows the observation of nano-objects suspended in a liquid phase, with a few manometers resolution and a good signal to noise ratio. The idea behind this technique is simply to perform STEM-in-SEM, that is SEM in transmission mode, in an environmental SEM. The purpose of the present contribution is to highlight the main advances that contributed to development of the wet-STEM technique. Although simple in principle, the wet-STEM imaging mode would have been limited before high brightness electron sources became available, and needed some progresses and improvements in ESEM. This new technique extends the scope of SEM as a high-resolution microscope, relatively cheap and widely available imaging tool, for a wider variety of samples.     

Variation of relative intensities between surface and bulk plasmon losses due to crystal orientations for aluminium in low energy electron reflection loss spectroscopy

The contrast change of secondary electron images due to the crystal orientations is observed by the ultra high vacuum scanning electron microscope (UHV-SEM) for crystal grains of clean surface of polycrystalline Al in the primary energy E_p of 200 eV to 5 keV. The low energy electron loss spectra are measured by the cylindrical mirror analyzer. The relative intensity ratio between surface and bulk plasmon loss spectra was dependent on the crystal orientations. The SEM images taken by the surface and bulk plasmon signals at E_p = 230 eV show the inverse contrast depending on the grains. The inversion of the relative intensities between the surface and bulk plasmon losses is explained qualitatively by taking into account of variation of the penetration depth of the incident beam caused by the electron channeling.     

One-pot solvothermal route to self-assembly of cauliflower-shaped CdS microspheres

Nearly monodispersed cauliflower-shaped CdS microspheres were prepared through a simple one-step solvothermal route on a large scale by employing sodium dodecyl sulfate (SDS) as the surfactant. Images by field emission scanning electron microscope (FESEM) and transmission electron microscope (TEM) indicate that cauliflower-shaped CdS microspheres with diameters in the range from 1.3 to 4.5 μm are assembled by nanoparticles with an average diameter of approximately 30 nm. The possible formation mechanism of the cauliflower-shaped CdS microspheres was also proposed. The photovoltaic activity of cauliflower-shaped CdS architectures has been investigated, indicating that the as-obtained CdS microspheres exhibited higher photovoltaic performance in comparison with CdS nanoparticles.     

合成温度对Ce掺杂SiC纳米线的制备及场发射性能的影响研究

本文利用化学气相反应(CVR)法, 系统研究了不同温度对Ce掺杂的SiC纳米线及其场发射性能的影响规律. 利用扫描电镜(SEM)、透射电镜(TEM)、选区电子衍射(SAED)、X射线衍射(XRD)对所得产物进行了表征, 并对其场发射性能进行了测试. 结果表明: 所得产物为具有立方结构的β-SiC晶体, 随着温度的升高, 纳米线逐渐变的弯曲, Ce的含量降低, 产物的开启电场和阈值电场先升高后降低. 当合成温度为1250 ℃, Ce的含量为0.27 at%, 产物的场发射性能最佳,开启电场和阈值电场分别为2.5 V/μm和5.2 V/μm. 关键词： 合成温度 SiC纳米线 场发射性能     

Determination of the linear attenuation range of electron transmission through film specimens

We have investigated the linear attenuation range of electron transmission through film specimens and its dependence on the electron energy, the acceptance half-angle of a detector or an objective aperture, and specimen properties, in the scanning transmission electron microscope (STEM) and the conventional transmission electron microscope (TEM). Electron transmission in the bright-field mode was calculated by the Monte Carlo simulation of electron scattering, and its range of the linear attenuation in film thickness was then determined by a linear least squares fit. The corresponding linear thickness range was shown to increase with the electron energy and the acceptance half-angle, although it decreased with the increase in the atomic number of specimen materials. Under the condition of a 300 kV STEM or a 3 MV ultra-high voltage electron microscope (ultra-HVEM), the linear attenuation range could extend to several microns for light specimen materials, and this was validated by experimental data in the ultra-HVEM. The presented results can be helpful for accurately measuring the specimen thickness or mass from electron transmission, and estimating the deviation of electron transmission from linearity when tilting a specimen in electron tomography.     

Morphology controlled solvothermal synthesis of Cd(OH)2 and CdO micro/nanocrystals on Cd foil

Cadmium hydroxide (Cd(OH)₂) and cadmium oxide (CdO) nano and micro crystals were synthesized in ethanol-water medium using cadmium foil both as a source and substrate under solvothermal condition. Different concentrations of ammonium hydroxide, hydrazine hydrate, sodium hydroxide and potassium hydroxide were added to study the structural and morphological variations in the products. Synthesis was carried out at different temperatures to study the growth stages of the nano/microstructures. The samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM). The as-prepared Cd(OH)₂ products were transformed to CdO by thermal treatment in air. The possible growth mechanism for the formation of different morphologies at different basic medium has been proposed. The optical absorption measurement was carried out to determine the values of the band gap of CdO.     

SEM扫描云纹法的相移技术研究

提出一种扫描电镜(SEM)扫描云纹法的相移新技术,通过SEM系统控制电镜电子束扫描线移动,对获取的云纹图像实现0-2π范围内的四步相移,从而获得了更高的位移测量灵敏度。同时对SEM扫描云纹法的测量原理以及相移实验技术的原理进行了详细的阐述。并将该技术应用到电子封装试件栅的相移分析中。实验结果证明了该方法的可行性,该方法为微米云纹法的条纹处理提供了一种新途径。     

In situ TEM and SEM studies on the antimicrobial activity and prevention of Candida albicans biofilm by Cassia spectabilis extract

The inhibitory effect of Cassia spectabilis methanol leaf extract was evaluated against biofilm forming Candida albicans, which was sensitive to 6.25 mg/ml concentration of the extract. Transmission (TEM) and scanning electron microscope (SEM) observations were used to study the anticandidal activity and prevention of biofilm formation by the C. spectabilis extract. SEM analysis further revealed reduction in C. albicans biofilm in response to the extract. The main abnormalities noted via TEM study was the alterations in morphology and complete collapse of the yeast cells after 36 h of exposure to the extract. The significant antifungal activity shown by this methanol extract of C. spectabilis suggests its potential against infections caused by C. albicans.