Sample scanning electron

Electron Microprobe Measurements. Compositional information regarding transpoirt 6T nickel and vanadium in the catalysts uppermost 10,000A surface layers was obtained from electron microprobe analysis of the samples. Scanning electron micrographs and x-ray spectra were obtained with a JEOL 733 scanning electron... 

Electron Beam Techniques. One of the most powerful tools in VLSI technology is the scanning electron microscope (sem) (see Microscopy). A sem is typically used in three modes secondary electron detection, back-scattered electron detection, and x-ray fluorescence (xrf). AH three techniques can be used for nondestmctive analysis of a VLSI wafer, where the sample does not have to be destroyed for sample preparation or by analysis, if the sem is equipped to accept large wafer-sized samples and the electron beam is used at low (ca 1 keV) energy to preserve the functional integrity of the circuitry. Samples that do not diffuse the charge produced by the electron beam, such as insulators, require special sample preparation. 

Asbestos fiber identification can also be achieved through transmission or scanning electron microscopy (tern, sem) techniques which are especially usefiil with very short fibers, or with extremely small samples (see Microscopy). With appropriate peripheral instmmentation, these techniques can yield the elemental composition of the fibers using energy dispersive x-ray fluorescence, or the crystal stmcture from electron diffraction, selected area electron diffraction (saed). 

In contrast to many other surface analytical techniques, like e. g. scanning electron microscopy, AFM does not require vacuum. Therefore, it can be operated under ambient conditions which enables direct observation of processes at solid-gas and solid-liquid interfaces. The latter can be accomplished by means of a liquid cell which is schematically shown in Fig. 5.6. The cell is formed by the sample at the bottom, a glass cover - holding the cantilever - at the top, and a silicone o-ring seal between. Studies with such a liquid cell can also be performed under potential control which opens up valuable opportunities for electrochemistry [5.11, 5.12]. Moreover, imaging under liquids opens up the possibility to protect sensitive surfaces by in-situ preparation and imaging under an inert fluid [5.13]. 

Perhaps the most significant complication in the interpretation of nanoscale adhesion and mechanical properties measurements is the fact that the contact sizes are below the optical limit ( 1 t,im). Macroscopic adhesion studies and mechanical property measurements often rely on optical observations of the contact, and many of the contact mechanics models are formulated around direct measurement of the contact area or radius as a function of experimentally controlled parameters, such as load or displacement. In studies of colloids, scanning electron microscopy (SEM) has been used to view particle/surface contact sizes from the side to measure contact radius [3]. However, such a configuration is not easily employed in AFM and nanoindentation studies, and undesirable surface interactions from charging or contamination may arise. For adhesion studies (e.g. Johnson-Kendall-Roberts (JKR) [4] and probe-tack tests [5,6]), the probe/sample contact area is monitored as a function of load or displacement. This allows evaluation of load/area or even stress/strain response [7] as well as comparison to and development of contact mechanics theories. Area measurements are also important in traditional indentation experiments, where hardness is determined by measuring the residual contact area of the deformation optically [8J. For micro- and nanoscale studies, the dimensions of both the contact and residual deformation (if any) are below the optical limit. 

Fig. 7.88 Scanning electron micrographs of cross-sections through interaction layers with superimposed Fe and Zn K, line scans across the layers (

The activity loss measured here is caused by recrystallizations. This was demonstrated by using scanning electron microscopy to determine nickel crystallite size in the same catalyst samples. These tests revealed that the catalyst used in demonstration plants has only a slight tendency to recrystallize or sinter after steam formation and loss of starting activity. 

The development and the recent increase in availability of the scanning electron microscope with its considerable depth of field and reduced beam intensity has widened the range of samples which can be examined... 

Replication avoids the problem of sample deterioration in the instrument, but it is destructive in that reaction of the material cannot be continued after the replica has been prepared. Transitory features cannot be detected unless a series of preparations are examined corresponding to increasing progress of the reaction considered. The textures of replicas have been shown [220] to be in satisfactory agreement with those of the original surface as viewed in the scanning electron microscope. The uses and interpretations of observations made through sample replication procedures are illustrated in the studies of decomposition of metal carboxyl-ates by Brown and co-workers [97,221—223]. 

Scanning electron microscopy and replication techniques provide information concerning the outer surfaces of the sample only. Accurate electron microprobe analyses require smooth surfaces. To use these techniques profitably, it is therefore necessary to incorporate these requirements into the experimental design, since the interfaces of interest are often below the external particle boundary. To investigate the zones of interest, two general approaches to sample preparation have been used. 

Figure 8.36. Scanning electron micrographs of an Ag-25at%Pd alloy electrode deposited on YSZ, (a,c,e) sample 1 (b, d, f) sample 2.39...

The results of the mechanical properties can be explained on the basis of morphology. The scanning electron micrographs (SEM) of fractured samples of biocomposites at 40 phr loading are shown in figure. 3. It can be seen that all the bionanofillers are well dispersed into polymer matrix without much agglomeration. This is due to the better compatibility between the modified polysaccharides nanoparticles and the NR matrix (Fig. 4A and B). While in case of unmodified polysaccharides nanoparticles the reduction in size compensates for the hydrophilic nature (Fig. 3C and D). In case of CB composites (Fig. 3E) relatively coarse, two-phase morphology is seen. 

FIGURE 3.14 Transmission electron microscopic (TEM) pictures of (a) acrylic rubber (ACM)-silica hybrid prepared from 1 1 tetraethoxysilane (TEOS)/water (H2O) and (b) 1 2 TEOS/H2O mole ratios and (c) scanning electron microscopic (SEM) picture of ACM-silica hybrid composite synthesized from 1 6 TEOS/H2O mole ratio. The concentration of TEOS has been kept constant at 45 wt% and the samples have been gelled at room temperature. (From Bandyopadhyay, A., De Sarkar, M., and Bhowmick, A.K., J. Appl. Polym. Sci., 95, 1418, 2005. Courtesy of Wiley InterScience.)... 

The authors wish to acknowledge the work of Paul McCarthy in scanning electron microscopy, Michael Saculla in x-ray radiography, and Steven Buckley and Chuck Chen in sample preparation and modulus measurement. This work was performed under the auspices of the U.S. Department of Energy by the Lawrence Livermore National Laboratory under Contract No. W-7405-ENG-48. 

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