Sem-Based Characterization Techniques

1986 ◽  
Vol 69 ◽  
Author(s):  
Phillip E. Russell

AbstractThe scanning electron microscope is now a common instrument in materials characterization laboratories. The basic role of the SEM as a topographic imaging system has steadily been expanding to include a wide variety of SEM-based analytical techniques. These techniques cover the range of basic semiconductor materials characterization to live-time device characterization of operating LSI or VLSI devices. This paper will introduce many of the more commonly used techniques, describe the modifications or additions to a conventional SEM required to utilize the techniques, and give examples of the use of such techniques. First, the types of signals available from a sample being irradiated by an electron beam will be reviewed. Then, where applicable, the type of spectroscopy or microscopy which has evolved to utilize the various signal types will be described. This will be followed by specific examples of the use of such techniques to solve problems related to semiconductor technology. Techniques to be emphasized will include: x-ray fluorescence spectroscopy, electron beam induced current (EBIC), stroboscopic voltage analysis, cathodoluminescence and electron beam IC metrology. Current and future trends of some of these techniques, as related to the semiconductor industry, will be discussed.

Author(s):  
R. E. Herfert

Studies of the nature of a surface, either metallic or nonmetallic, in the past, have been limited to the instrumentation available for these measurements. In the past, optical microscopy, replica transmission electron microscopy, electron or X-ray diffraction and optical or X-ray spectroscopy have provided the means of surface characterization. Actually, some of these techniques are not purely surface; the depth of penetration may be a few thousands of an inch. Within the last five years, instrumentation has been made available which now makes it practical for use to study the outer few 100A of layers and characterize it completely from a chemical, physical, and crystallographic standpoint. The scanning electron microscope (SEM) provides a means of viewing the surface of a material in situ to magnifications as high as 250,000X.


Author(s):  
J. I. Bennetch

In a recent study of the superplastic forming (SPF) behavior of certain Al-Li-X alloys, the relative misorientation between adjacent (sub)grains proved to be an important parameter. It is well established that the most accurate way to determine misorientation across boundaries is by Kikuchi line analysis. However, the SPF study required the characterization of a large number of (sub)grains in each sample to be statistically meaningful, a very time-consuming task even for comparatively rapid Kikuchi analytical techniques.In order to circumvent this problem, an alternate, even more rapid in-situ Kikuchi technique was devised, eliminating the need for the developing of negatives and any subsequent measurements on photographic plates. All that is required is a double tilt low backlash goniometer capable of tilting ± 45° in one axis and ± 30° in the other axis. The procedure is as follows. While viewing the microscope screen, one merely tilts the specimen until a standard recognizable reference Kikuchi pattern is centered, making sure, at the same time, that the focused electron beam remains on the (sub)grain in question.


Author(s):  
L. T. Germinario

Understanding the role of metal cluster composition in determining catalytic selectivity and activity is of major interest in heterogeneous catalysis. The electron microscope is well established as a powerful tool for ultrastructural and compositional characterization of support and catalyst. Because the spatial resolution of x-ray microanalysis is defined by the smallest beam diameter into which the required number of electrons can be focused, the dedicated STEM with FEG is the instrument of choice. The main sources of errors in energy dispersive x-ray analysis (EDS) are: (1) beam-induced changes in specimen composition, (2) specimen drift, (3) instrumental factors which produce background radiation, and (4) basic statistical limitations which result in the detection of a finite number of x-ray photons. Digital beam techniques have been described for supported single-element metal clusters with spatial resolutions of about 10 nm. However, the detection of spurious characteristic x-rays away from catalyst particles produced images requiring several image processing steps.


2019 ◽  
Vol 34 (5) ◽  
pp. 854-859 ◽  
Author(s):  
Sofia Pessanha ◽  
Sara Silva ◽  
Luís Martins ◽  
José Paulo Santos ◽  
João M. Silveira

In this work, we established a methodology for the analysis and characterization of hydroxyapatite-based materials using X-ray fluorescence.


2012 ◽  
Vol 48 (2) ◽  
pp. 281-290 ◽  
Author(s):  
Noely Camila Tavares Cavalcanti ◽  
Giovana Damasceno Sousa ◽  
Maria Alice Maciel Tabosa ◽  
José Lamartine Soares Sobrinho ◽  
Leila Bastos Leal ◽  
...  

The aim of this study was to characterize three batches of albendazole by pharmacopeial and complementary analytical techniques in order to establish more detailed specifications for the development of pharmaceutical forms. The ABZ01, ABZ02, and ABZ03 batches had melting points of 208 ºC, 208 ºC, and 209 ºC, respectively. X-ray diffraction revealed that all three batches showed crystalline behavior and the absence of polymorphism. Scanning electron microscopy showed that all the samples were crystals of different sizes with a strong tendency to aggregate. The samples were insoluble in water (5.07, 4.27, and 4.52 mg mL-1, respectively) and very slightly soluble in 0.1 M HCl (55.10, 56.90, and 61.70 mg mL-1, respectively) and additionally showed purities within the range specified by the Brazilian Pharmacopoeia 5th edition (F. Bras. V; 98% to 102%). The pharmacopeial assay method was not reproducible and some changes were necessary. The method was validated and showed to be selective, specific, linear, robust, precise, and accurate. From this characterization, we concluded that pharmacopeial techniques alone are not able to detect subtle differences in active pharmaceutical ingredients; therefore, the use of other complementary techniques is required to ensure strict quality control in the pharmaceutical industry.


2021 ◽  
Vol 10 (1) ◽  
pp. 1
Author(s):  
Jianhui Wu ◽  
Cailian Du ◽  
Jieming Zhang ◽  
Bo Yang ◽  
Andrew G. S. Cuthbertson ◽  
...  

Nanotechnology is increasingly being used in areas of pesticide production and pest management. This study reports the isolation and virulence of a new Metarhizium anisopliae isolate SM036, along with the synthesis and characterization of M. anisopliae–chitosan nanoparticles followed by studies on the efficacy of nanoparticles against Plutella xylostella. The newly identified strain proved pathogenic to P. xylostella under laboratory conditions. The characterization of M. anisopliae–chitosan nanoparticles through different analytical techniques showed the successful synthesis of nanoparticles. SEM and HRTEM images confirmed the synthesis of spherical-shaped nanoparticles; X-ray diffractogram showed strong peaks between 2θ values of 16–30°; and atomic force microscopy (AFM) analysis revealed a particle size of 75.83 nm for M. anisopliae–chitosan nanoparticles, respectively. The bioassay studies demonstrated that different concentrations of M. anisopliae–chitosan nanoparticles were highly effective against second instar P. xylostella under laboratory and semi-field conditions. These findings suggest that M. anisopliae–chitosan nanoparticles can potentially be used in biorational P. xylostella management programs.


2021 ◽  
Vol 234 ◽  
pp. 00106
Author(s):  
Houda Labjar ◽  
Hassan Chaair

The synthesis of apatite silicated Ca10(PO4)6-x(SiO4)x(OH)2-x (SiHA) with 0≤x≤2 was investigated using a wet precipitation method followed by heat treatment using calcium carbonate CaCO3 and phosphoric acid H3PO4 and silicon tetraacetate SiC8H20O4 (TEOS) in medium of water ethanol, with three different silicate concentrations. After drying, the samples are ground and then characterized by different analytical techniques like X-ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR) and Scanning electron Microscopy (SEM) and chemical analysis.


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