A new method for low-magnification in the environmental scanning electron microscope

A device has been developed and used successfully on two models of the environmental scanning electron microscope that allows low-magnification imaging of about 30x, significantly better than the original 200x low-magnification imaging limit. This was achieved by using an additional aperture to limit the pressure at a point where it will not block the electron beam, and a larger aperture plate for the combination final aperture/secondary electron signal collection surface that also does not block the electron beam significantly.     

Applications of the environmental scanning electron microscope to the analysis of pharmaceutical formulations

Electron microscopy has been used for several years as a routine tool for the study of pharmaceutical formulations. However, it is usually desirable to obtain information on these systems in the wet state, and there are concerns regarding the interpretation of information provided by conventional electron microscopy where samples are subjected to preparation techniques which may include freezing, drying, fracturing, and coating. The environmental scanning electron microscope (ESEM) has been used to analyse a number of pharmaceutical samples in their natural state. Results obtained from these samples, including biodegradable matrices, microparticulate systems (both degradable and non-biodegradable), and bioadhesive matrices, will be discussed and the merits and limitations of the ESEM will be highlighted.     

The role of induced contrast in images obtained using the environmental scanning electron microscope

Generation of contrast in images obtained using the environmental scanning electron microscope (ESEM) is explained by interpretation of images acquired using the gaseous secondary electron detector (GSED), ion current, and the Everhart-Thornley detector. We present a previously unreported contrast component in GSED and ion current images attributed to signal induction by changes in the concentration of positive ions in the ESEM chamber during image acquisition. Changes in positive ion concentration are caused by changes in electron emission from the sample during image acquisition and by a discrepancy between the drift velocities of negative and positive charge carriers in the imaging gas. The proposed signal generation mechanism is used to explain contrast reversal in images produced using the GSED and ion current signals and accounts for discrepancies in contrast observed, under some conditions, in these types of images. Combined with existing models of signal generation in the ESEM, the proposed model provides a basis for correct interpretation of ESEM images.     

Some aspects of optimizing contrasts for the investigation of joint materials in the environmental scanning electron microscope

In the environmental scanning electron microscope, material joints of different atomic mass and different electrical conducting properties can easily be observed simultaneously without coating the specimen. For such heterogeneous materials, the quality of the image can be optimized with respect to contrast and resolution if the contrast types as well as their significance to the composition of the image are known.     

Tensile tests of polymers at low temperatures in the environmental scanning electron microscope: an improved cooling platform

The investigation of the fracture behavior of polymers in the environmental scanning electron microscope (ESEM) can provide information about the correlation between the microstructure of a specimen and the macroscopic stress-strain characteristic. As the mechanical properties of polymers change dramatically at the glass transition temperature, cooling of the specimens during the tensile tests can yield very valuable information about the influence of individual components of polymer blends on the fracture behavior of the material. A serious problem in this connection is the poor heat conductivity of polymers. A commercially available cooling platform, which can be mounted on the tensile stage used for the tests was substantially modified to both enhance the heat transfer between platform and specimen, and to minimize the temperature gradient along the specimen.The first experiments on modified polypropylene specimens already delivered some unexpected results. Fibril-like structures appeared at the crack tip that would not be expected at temperatures below the glass transition temperature of the polymer blend.     

Quantitative secondary ion mass spectrometry imaging of self-assembled monolayer films for electron beam dose mapping in the environmental scanning electron microscope

Fluorinated alkanethiol self-assembled monolayers (SAM) films immobilized on gold substrates have been used as electron-sensitive resists to map quantitatively the spatial distribution of the primary electronbeam scattering in an environmental scanning electron microscope (ESEM). In this procedure, a series of electron dose standards are prepared by exposing a SAM film to electron bombardment in well-defined regions at different levels of electron dose. Microbeam secondary ion mass spectrometry (SIMS) using Cs⁺ bombardment is then used to image the F^- secondary ion signal from these areas. From the reduction in F^- intensity as a function of increasing electron dose, a calibration curve is generated that allows conversion of secondary ion signal to electron dose on a pixel-by-pixel basis. Using this calibration, electron dose images can be prepared that quantitatively map the electron scattering distribution in the ESEM with micrometer spatial resolution. The SIMS imaging technique may also be used to explore other aspects of electron-surface interactions in the ESEM.     

The effect of some instrument operating conditions on the x-ray microanalysis of particles in the environmental scanning electron microscope

The objective of this investigation was to evaluate the practical effects of electron beam broadening in the environmental scanning electron microscope (ESEM) on particle x-ray microanalysis and to determine some of the optimum operating conditions for this type of analysis. Four sets of experiments were conducted using a Faraday cage and particles of copper, glass, cassiterite, andrutile. The accelerating voltage and chamber pressure varied from 20 to 10 kV and from 665–66 Pa (5.0 to 0.5 torr), respectively. The standard gaseous secondary electron detectors (GSED) and the long environmental secondary dectectors (ESD) for the ESEM were evaluated at different working distances. The effect of these parameters on the presence of artifact peaks was evaluated. The particles were mounted on carbon tape on an aluminum specimen mount and were analyzed individually and as a mixture. Substrate peaks were present in almost all of the spectra. The presence of neighboring particle peaks and the number of counts in these depended upon the operating conditions. In general, few of these peaks were observed with the long ESD detector at 19 mm working distance and at low chamber pressures. More peaks and counts were observed with a deviation from these conditions. The most neighboring peaks and counts were obtained with the GSED detector at 21.5 mm working distance, 10 kV accelerating voltage, and 665 Pa (5.0 torr) chamber pressure. The results of these experiments support the idea that the optimum instrumental operating conditions for EDS analysis in the ESEM occur by minimizing the gas path length and the chamber water vapor pressure, and by maximizing the accelerating voltage. The results suggest that the analyst can expect x-ray counts from the mounting materials. These tests strongly support the recommendation of the manufacturer to use the long ESD detector and a 19 mm working distance for EDS analysis. The results of these experiments indicate that neighboring particles millimeters from the target may contribute x-ray counts to the spectrum.     

Some theoretical aspects of type-1 magnetic contrast in the scanning electron microscope

Type-1 magnetic contrast can be obtained in the secondary electron (SE) image in the SEM from a sample having an external magnetic field if the SE detector is directionally sensitive. Gauss' theorem is applied to show that the normal component of induction at the surface of the sample can be calculated from the measured spatial derivative(s) of the SE difference-signal. A method is given in this paper for calculating the three components of the induction in the entire volume above the sample surface. Reasons are given for believing that type-1 magnetic contrast is limited in spatial resolution by the fluxon unit.     

X-ray microanalysis of wet biological specimens in the environmental scanning electron microscope. 1. Reduction of specimen distance under different atmospheric conditions

X-ray microanalysis of non-biological and biological specimens was carried out in the environmental scanning electron microscope (ESEM) under different conditions of specimen distance (the distance travelled by the electron probe within the specimen chamber) and chamber atmosphere. Using both water vapour and argon atmospheres, it was shown that reduction in specimen distance had no effect on atmospheric gas X-ray signal in either case. Unlike water vapour, increased levels of argon (up to 10 torr) caused a marked depression of specimen P/B ratios, with a decrease in both characteristic and background (continuum) counts. These effects in argon were not altered by reduction in specimen distance. Specimen distance was important in relation to beam skirting and elemental analysis. With an extended assembly (short specimen distance), beam skirting in a water-vapour atmosphere was much reduced – leading to enhanced element detectability in a discrete biological specimen (Anabaena cyclindrica).