Advanced Nano-Scale Metrology for the Characterization of Ceramic Materials in the Scanning Electron Microscope

2008 ◽  
Vol 606 ◽  
pp. 93-101
Author(s):  
Giuseppe Pezzotti ◽  
Atsuo Matsutani ◽  
Maria Chiara Munisso ◽  
Wen Liang Zhu

With the proliferation of several types and classes of high performance ceramic materials, the screening, evaluation and integration of new materials into structures and devices require a new and more effective approach. Evaluation on the nano-scale of the mechanical characteristics of new ceramic materials requires multiple complementary metrology tools. We report here about an advanced metrology tool, cathodoluminescence (CL) spectroscopy, which has a potential to rapidly screen and evaluate residual stress characteristics in advanced ceramic materials and structures. Nano-scale stress measurements are made in situ into an integrated metrology vacuum chamber in a field-emission gun scanning electron microscope (FEG-SEM). Complementing this tool, we also describe a new image analysis based on CL emission for fast screening and ranking of domain structures in ferroelastic ceramics. The end result of this paper is to show how crystallographic and mechanical characteristics of ceramics can be quantitatively characterized in a hybrid device combining electro-stimulated imaging and spectroscopic outputs.

Author(s):  
Marc H. Peeters ◽  
Max T. Otten

Over the past decades, the combination of energy-dispersive analysis of X-rays and scanning electron microscopy has proved to be a powerful tool for fast and reliable elemental characterization of a large variety of specimens. The technique has evolved rapidly from a purely qualitative characterization method to a reliable quantitative way of analysis. In the last 5 years, an increasing need for automation is observed, whereby energy-dispersive analysers control the beam and stage movement of the scanning electron microscope in order to collect digital X-ray images and perform unattended point analysis over multiple locations.The Philips High-speed Analysis of X-rays system (PHAX-Scan) makes use of the high performance dual-processor structure of the EDAX PV9900 analyser and the databus structure of the Philips series 500 scanning electron microscope to provide a highly automated, user-friendly and extremely fast microanalysis system. The software that runs on the hardware described above was specifically designed to provide the ultimate attainable speed on the system.


1986 ◽  
Vol 25 (Part 2, No. 9) ◽  
pp. L758-L760 ◽  
Author(s):  
Kazuyuki Koike ◽  
Hideo Matsuyama ◽  
Katsuya Mitsuoka ◽  
Kazunobu Hayakawa

2006 ◽  
Vol 309-311 ◽  
pp. 1215-1218
Author(s):  
Kiyotaka Yamada ◽  
Junji Ikeda ◽  
Giuseppe Pezzotti

The electro-stimulated luminescence spectrum of a rare-earth ion added to zirconia (ZrO2) lattice was investigated with the aim of using it as a sensor for nano-scale stress (fluorescence piezo-spectroscopy) and phase transformation assessments in a field emission scanning electron microscope (FE-SEM). In this paper, the selected rare-earth fluorescent ion Eu, added to ZrO2 as a raw oxide powder (Eu2O3) before sintering (in the amount of 1.0 wt. %). Spectroscopic results indicated that the spectral shift of some fluorescent band of the selected rare-earth ion was sensitive to residual stress and that the electron-stimulated spectra of Eu2O3-doped ZrO2 in its tetragonal and monoclinic polymorphs were different to each other. Based on these findings, the luminescent substance can be useful as a “stress and phase transformation sensor”, in order to clarify the elementary mechanisms behind synthetic ZrO2.


2021 ◽  
pp. 67-75

Eight historical textile objects belonging to the 16th-20th centuries in the collection of the Topkapi Palace Museum in Istanbul were analyzed with the purpose of reaching improved conservation and restoration methods. The historical textiles underwent dyestuff analysis by High Performance Liquid Chromatography, morphological and elemental analysis by Scanning Electron Microscope with energy Dispersive X-ray Spectroscopy, CIEL*a*b color measurement as well as technical analysis by optical microscopy.


Author(s):  
V.G. Macres ◽  
O. Preston ◽  
N.C. Yew ◽  
R. Buchanan

The instrument described here is the Materials Analysis Company Model 400S combined scanning electron microscope/electron micro-probe analyzer. It was designed specifically to incorporate the most advanced features of a high performance electron microprobe analyzer with those of a medium resolution (1000A°) scanning electron microscope. The high effective x-ray take-off angle of the instrument (38.5°) offers low x-ray absorption, and thus allows the analysis of fairly rough specimens. The large depth of focus of the scanned electron images further enhances the capability of examining rough specimens.The electron-optical column comprises a triode electron gun, double condenser lens and objective lens. The electron gun uses a conventional hairpin filament, autobiased Wehnelt cylinder and anode. An externally controlled filament/Wehnelt cylinder height adjustment is provided for optimizing gun performance at all operating potentials. The double condenser lens is unitized and has two lens regions and a common energizing coil.


Author(s):  
Var L. St. Jeor ◽  
C. C. Chau ◽  
Mark Thomsen

A large portion of the interest currently given high performance polymer fibers stems from their potential use in composite construction. Although many of these fibers display good tensile properties, compressive strength is a major concern. There are many studies which have observed the compressive failure morphology of polymeric fibers. These studies usually involve the postmortem observation of samples which have failed, either partly or completely, following compressive strain. Observations have included such events as kink band formation, brittle failure and other modes as well. But to our knowledge these failure modes have not been recorded, in process, using the scanning electron microscope (SEM). In this article we introduce a technique which allows observation of compressive failure within the SEM, or using light microscopy (LM), in process. We also present some results unique to this procedure. This technique allows us to follow this "process" of compressive failure including both it's initiation and the more advanced stages of failure. Since the compressive failure of polymeric fibers is a process rather than an instantaneous event we have been able to record this process of failure, in it's various stages, in relatively high resolution SEM micrographs. Our methodology involves the use of relatively low accelerating voltages to minimize charging artifacts associated with damaged areas of the fiber. This induced damage can disrupt the 3 - 5nm sputter coating used to prevent such artifact resulting in uncoated fiber being exposed to the electron beam. This technique also lends itself readily to video recording. We have observed compressive failure processes for Kevlar 49®, Spectra 1000®, Hercules AS-4® carbon and various experimental fibers such as Polybenzobisoxazole (PBO). Our observations have included such modes of failure as kink band formation, delamination, buckling and brittle failure. It is noted that some of these processes occur simultaneously in any given fiber, and with the exception of brittle failure, these processes can be recorded at every stage of development visible to the SEM.


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