扫描电镜的最新发展——低电压扫描电镜（LVSEM）和扫描低能电镜（SLEEM）

本文从仪器和电子光学的观点评述了在扫描电镜上的装备场发射枪以后,向低电压扫描电镜和扫描低能电镜发展中的一些重要问题。讨论了低能和极低能时二次电子和背散射电子的特性,低电压扫描电镜作扫描低能电镜能量段的划分,实现低电压扫描电镜和扫抵低能电镜的困难,以及利用阻场透镜的解决办法。讨论了低能情形下信号的探测,杂散电磁场的影响的估计和仪器的分辨率。     

Secondary electron hyperspectral imaging: nanostructure and chemical analysis for the LV-SEM

ABSTRACT

Materials engineers have increasing control over nanoscale chemical composition and nanostructures. The latter can be easily analysed by the scanning electron microscope (SEM) yet nanoscale chemical analysis in the SEM poses challenges. Nevertheless, nanoscale chemical analysis capabilities have been developed in the LV-SEM by secondary electron hyperspectral imaging (SEHI). In this article, the insights that SEHI has provided into well characterised semiconductor, photovoltaic, polymer and hard carbon materials are reviewed. Instrument and experimental considerations for the obtainment of secondary electron hyper-spectra are discussed and recommendations for future analyses in the LV-SEM by SEHI are made.     

Solid state NMR and LVSEM studies on the hardening of latex modified tile mortar systems

Construction mortars contain a broad variety of both inorganic and organic additives beside the cement powder. Here we present a study of tile mortar systems based on portland cement, quartz, methyl cellulose and different latex additives. As known, the methyl cellulose stabilizes the freshly prepared cement paste, the latex additive enhances final hydrophobicity, flexibility and adhesion. Measurements were performed by solid state nuclear magnetic resonance (NMR) and low voltage scanning electron microscopy (LVSEM) to probe the influence of the latex additives on the hydration, hardening and the final tile mortar properties. While solid state NMR enables monitoring of the bulk composition, scanning electron microscopy affords visualization of particles and textures with respect to their shape and the distribution of the different phases.

Within the alkaline cement paste, the poly(vinyl acetate) (VAc)-based latex dispersions stabilized by poly(vinyl alcohol) (PVA) were found to be relatively stable against hydrolysis. The influence of the combined organic additives methyl cellulose, poly(vinyl alcohol) and latexes stabilized by poly(vinyl alcohol) on the final silicate structure of the cement hydration products is small. But even small amounts of additives result in an increased ratio of ettringite to monosulfate within the final hydrated tile mortar as monitored by ²⁷Al NMR. The latex was found to be adsorbed to the inorganic surfaces, acting as glue to the inorganic components. For similar latex water interfaces built up by poly(vinyl alcohol), a variation in the latex polymer composition results in modified organic textures. In addition to the networks of the inorganic cement and of the latex, there is a weak network build up by thin polymer fibers, most probably originating from poly(vinyl alcohol). Besides the weak network, polymer fibers form well-ordered textures covering inorganic crystals such as portlandite.     

Electrodeposition of organofunctional silanes and its influence on structural adhesive bonding

Four different organofunctional silanes were selected and deposited on chemically pretreated aluminum surfaces by immersion and electrodeposition techniques. The surface morphology, comparison of elemental constituents, and surface free energies of silane-coated aluminum were investigated by low voltage scanning electron microscopy (LVSEM), low voltage X-ray analysis (LVXA), and contact angle measurement, respectively. The initial bond strength and long-term durability were evaluated with epoxy adhesive by lap shear tests. The deposition of silane coupling agents enhanced the bond durability of aluminum/epoxy joints under heat and humidity conditions. Also the performance of silane coupling agents depended on the application method. The electrodeposition technique produced a more uniform coverage of silane on the aluminum surface and, thus, was generally more effective than the immersion technique in improving bond performance.     

MgCl2负载催化剂和低产率聚合物样品形貌的LVSEM表征

采用低压扫描电子显微镜(LVSEM)表征了MgCl2负载的zjegler-Natta催化剂和极低产率聚丙烯颗粒的形貌.MgCl2时空气十分敏感,暴露在空气中十几秒就足以影响催化荆的形貌.LVSEM可以在低的入射电压(如l keV)下就得到高分辨率的图像.在低入射电压下,样品表面不会产生电荷积累.因此无需对样品进行喷涂导电层处理.由于极大地缩短了与空气的接触时间,LVSEM可以避免空气对样品形貌的干扰,成为表征Mgcl2负栽催化剂形貌的有力手段.     

Influence of the angular distribution of backscattered electrons on signals at different take-off angles in low-voltage scanning electron microscopy (LVSEM)

It is well known that the differential Mott cross section for large-angle elastic scattering shows maxima and minima at angles depending on material and electron energy. For electron energies of 10–30 keV, the averaging by frequent elastic scattering processes results in approximate Lambert angular distributions of backscattered electrons (BSE). However, the present Monte Carlo calculations for electron energies E = 1–5 keV and different angles of incidence show strong deviations from a Lambert distribution which increases with decreasing energy. The signals of the BSE detector with five annular segments for different take-off directions show good agreement with the calculations for normal electron incidence.     

Beam transfer characteristics of a commercial environmental SEM and a low vacuum SEM

Two commercial instruments that permit a gaseous environment in their specimen chamber have been investigated, namely, a 'FEI Quanta 600 FEG' environmental scanning electron microscope and a 'LEO SUPRA 35VP FESEM' low vacuum scanning electron microscope. The gas flow field is first computed by the direct simulation Monte Carlo method and the gas density gradient, speed, Mach number and temperature are found in the transition region from high pressure to vacuum. The electron beam transfer characteristics are then derived for different accelerating voltages and pressures and a comparison is made among different situations and with some published works. Certain physical parameters are analysed and discussed to establish a figure of merit that can be used as a standard performance specification for commercial environmental scanning electron microscope and low vacuum scanning electron microscope.     

Nascent morphology of polyethylene polymerized on flat model catalysts

The morphology and the thermal behavior of nascent polyethylene (PE) polymerized on flat models for the Phillips CrO_x/SiO₂ catalyst were investigated using low‐voltage scanning electron microscopy (LVSEM) and differential scanning calorimetry (DSC). Ethylene polymerizations were performed at 25 °C and 70 °C in gas phase. For the applied polymerization conditions, microscopy observations reveal that the formation of the macromolecules at the active catalyst sites, and their subsequent crystallization on the catalyst, result in homogeneous polymer layers having a thickness of the order of micrometers. The surface morphology of the nascent samples consists of spherical entities having a diameter less than one micrometer. Pillar‐like objects form the internal structure of the PE films. Because these entities are only loosely connected, high porosity is observed within the entire film. Thermal analysis of the samples shows that melting temperature and crystallinity of the nascent PE samples polymerized at 25 °C are noticeably higher than after melting and recrystallization. Samples polymerized at 70 °C, however, do not show these features. Copyright © 2004 Society of Chemical Industry