Sample Preparation Techniques for Grain Boundary Characterization of Annealed TRISO-Coated Particles

Silica due to its large inorganic amorphous wall and hydrophilic surface properties renders its suitability for designing different varieties of organic–inorganic silica-based materials. Characterization of such hybrid silica-based materials is one of the fascinating as well as challenging topics to be covered. Surface analysis of these hybrid materials can be done utilizing various techniques, out of which X-ray photoelectron spectroscopy (XPS), 29Si Solid-state Nuclear magnetic resonance (NMR) spectroscopy, and Fourier-transform infrared spectroscopy (FTIR) is the most ideal ones. Thus, before analyzing these silica materials, it requires a massive study on its sample preparation for appropriate characterization of the organic molecules present in the inorganic network. Hence, this chapter will give a brief elucidation of the sample preparation techniques for analyzing the hybrid materials utilizing the above instrumentation techniques.

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Sample preparation techniques for nano-mechanical characterization of glass fiber reinforced polyester matrix composites

Composites Part A Applied Science and Manufacturing ◽

10.1016/s1359-835x(02)00231-2 ◽

2003 ◽

Vol 34 (1) ◽

pp. 53-65 ◽

Cited By ~ 22

Author(s):

Sanjeev K. Khanna ◽

Robb M. Winter ◽

P. Ranganathan ◽

S.B. Yedla ◽

M. Kalukanimuttam ◽

...

Keyword(s):

Sample Preparation ◽

Glass Fiber ◽

Mechanical Characterization ◽

Matrix Composites ◽

Fiber Reinforced ◽

Glass Fiber Reinforced ◽

Polyester Matrix ◽

Preparation Techniques

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Improving transmission electron microscopy characterization of semiconductors by minimizing sample preparation artifacts

Canadian Journal of Physics ◽

10.1139/p92-138 ◽

1992 ◽

Vol 70 (10-11) ◽

pp. 875-880 ◽

Cited By ~ 6

Author(s):

J. P. McCaffrey ◽

G. I. Sproule ◽

R. Sargent

Keyword(s):

Electron Microscopy ◽

Transmission Electron Microscopy ◽

Sample Preparation ◽

Ion Milling ◽

Transmission Electron ◽

Transmission Electron Microscopy Characterization ◽

Silicon Based ◽

Microscopy Characterization ◽

Preparation Techniques

Techniques employed for the preparation of transmission electron microscopy (TEM) samples can introduce artifacts that obscure subtle detail in the materials being studied. Traditional semiconductor sample preparation techniques rely heavily on ion milling, which leaves amorphous layers on ion milled surfaces and some intermixing across interfaces, thus degrading the TEM images of these samples. Experimental results of the extent of this amorphization and intermixing are presented for silicon-based semiconductor samples, and methods to minimize these effects are suggested. These methods include variations in ion milling parameters that reduce the extent of the artifacts, and improvements in the small-angle cleavage technique that eliminate these artifacts completely.

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TEM Sample Preparation: An Interdisciplinary Website

Microscopy Today ◽

10.1017/s1551929500054481 ◽

2009 ◽

Vol 17 (2) ◽

pp. 38-41 ◽

Cited By ~ 1

Author(s):

Jeanne Ayache ◽

Luc Beaunier ◽

Jacqueline Boumendil ◽

Gabrielle Ehret ◽

Danièle Laub

Keyword(s):

Electron Microscopy ◽

Transmission Electron Microscopy ◽

Sample Preparation ◽

Material Science ◽

International Community ◽

Central Importance ◽

Transmission Electron ◽

Characterization Of Materials ◽

Preparation Techniques

Sample preparation is of central importance for the characterization of materials by transmission electron microscopy (TEM). As a guide to researchers seeking practical help on the use of all types of TEM sample preparation techniques, we have created an Internet website. This website has been designed in French and is now translated into English. The website is accessible free of charge.The TEMSAMPREP website, figure 1 http://temsamprep.in2p3.fr/, is the result of a synergistic effort of an atypical team of five electron microscopy scientists having different research specialties in physics, mineralogy, material science, and biology. They shared five years of human adventure in creating the website to transmit their 30 years of TEM experience to the international community.

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Nanomechanical Characterization of Cement-Based Materials

Advances in Environmental Engineering and Green Technologies - Nanotechnology Applications for Improvements in Energy Efficiency and Environmental Management ◽

10.4018/978-1-4666-6304-6.ch002 ◽

2015 ◽

pp. 41-55

Author(s):

Salim Barbhuiya

Keyword(s):

Mechanical Properties ◽

Data Analysis ◽

Sample Preparation ◽

Elastic Properties ◽

Nanomechanical Properties ◽

Cement Based Materials ◽

Properties Of Materials ◽

Preparation Techniques

Nanoindentation technique is used to assess the mechanical properties of materials at nano-level. A very small tip (usually diamond) produces indents at the surface of the material to be tested. A load vs. deflection curve is generated and is used to study the elastic properties of materials. Generally, it is used for obtaining the hardness and Young's modulus of materials at nano-meter scale. Currently, the method to evaluate the mechanical properties by nanoindentation is restricted to homogeneous materials. Cement-based materials are heterogeneous in nature. Therefore, nanoindentation study of cement-based materials is critical and requires several important steps, which need to be performed accurately. This chapter provides a review of the theory of nanoindentation, instruments being used for nanoindentation, sample preparation techniques, indentation strategy, and determination of nanomechanical properties and data analysis for cement-based materials.

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A Freeze Shadow Technique for the Preparation of Soft Paint Latexes for Electron Microscopy

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100079097 ◽

1977 ◽

Vol 35 ◽

pp. 314-315

Author(s):

Earl R. Walter ◽

Glen H. Bryant

Keyword(s):

Sample Preparation ◽

High Vacuum ◽

Vacuum System ◽

Latex Particles ◽

New Methods ◽

Diffusion Pump ◽

Film Forming ◽

Routine Basis ◽

Distribution Studies ◽

Preparation Techniques

With the development of soft, film forming latexes for use in paints and other coatings applications, it became desirable to develop new methods of sample preparation for latex particle size distribution studies with the electron microscope. Conventional latex sample preparation techniques were inadequate due to the pronounced tendency of these new soft latex particles to distort, flatten and fuse on the substrate when they dried. In order to avoid these complications and obtain electron micrographs of undistorted latex particles of soft resins, a freeze-dry, cold shadowing technique was developed. The method has now been used in our laboratory on a routine basis for several years.The cold shadowing is done in a specially constructed vacuum system, having a conventional mechanical fore pump and oil diffusion pump supplying vacuum. The system incorporates bellows type high vacuum valves to permit a prepump cycle and opening of the shadowing chamber without shutting down the oil diffusion pump. A baffeled sorption trap isolates the shadowing chamber from the pumps.

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Cryomicroscopy of multiphase latices

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100089615 ◽

1991 ◽

Vol 49 ◽

pp. 1060-1061

Author(s):

O. L. Shaffer ◽

M.S. El-Aasser ◽

C. L. Zhao ◽

M. A. Winnik ◽

R. R. Shivers

Keyword(s):

Electron Microscopy ◽

Radiation Damage ◽

Freeze Fracture ◽

Particle Morphology ◽

Second Stage ◽

Transmission Electron ◽

Important Approach ◽

Carbon Coated ◽

Preparation Techniques

Transmission electron microscopy is an important approach to the characterization of the morphology of multiphase latices. Various sample preparation techniques have been applied to multiphase latices such as OsO4, RuO4 and CsOH stains to distinguish the polymer phases or domains. Radiation damage by an electron beam of latices imbedded in ice has also been used as a technique to study particle morphology. Further studies have been developed in the use of freeze-fracture and the effect of differential radiation damage at liquid nitrogen temperatures of the latex particles embedded in ice and not embedded.Two different series of two-stage latices were prepared with (1) a poly(methyl methacrylate) (PMMA) seed and poly(styrene) (PS) second stage; (2) a PS seed and PMMA second stage. Both series have varying amounts of second-stage monomer which was added to the seed latex semicontinuously. A drop of diluted latex was placed on a 200-mesh Formvar-carbon coated copper grid.

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Characterization of intergranular cuprous oxide in polycrystalline YBa2Cu3O7-x

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100106466 ◽

1988 ◽

Vol 46 ◽

pp. 880-881

Author(s):

Bradley L. Thiel ◽

Chan Han R. P. ◽

Kurosky L. C. Hutter ◽

I. A. Aksay ◽

Mehmet Sarikaya

Keyword(s):

Grain Boundary ◽

Cuprous Oxide ◽

Room Temperature ◽

Boundary Phase ◽

Spectroscopic Techniques ◽

Transition Width ◽

Practical Applications ◽

Thin Foils ◽

Superconducting Oxides

The identification of extraneous phases is important in understanding of high Tc superconducting oxides. The spectroscopic techniques commonly used in determining the origin of superconductivity (such as RAMAN, XPS, AES, and EXAFS) are surface-sensitive. Hence a grain boundary phase several nanometers thick could produce irrelevant spectroscopic results and cause erroneous conclusions. The intergranular phases present a major technological consideration for practical applications. In this communication we report the identification of a Cu2O grain boundary phase which forms during the sintering of YBa2Cu3O7-x (1:2:3 compound).Samples are prepared using a mixture of Y2O3. CuO, and BaO2 powders dispersed in ethanol for complete mixing. The pellets pressed at 20,000 psi are heated to 950°C at a rate of 5°C per min, held for 1 hr, and cooled at 1°C per min to room temperature. The samples show a Tc of 91K with a transition width of 2K. In order to prevent damage, a low temperature stage is used in milling to prepare thin foils which are then observed, using a liquid nitrogen holder, in a Philips 430T at 300 kV.

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Advanced TEM sample preparation techniques for submicron Si devices

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100138956 ◽

1995 ◽

Vol 53 ◽

pp. 516-517 ◽

Cited By ~ 1

Author(s):

P. B. Basham ◽

H. L. Tsai

Keyword(s):

Sample Preparation ◽

Process Development ◽

Light Transmission ◽

Specific Area ◽

Turnaround Time ◽

Small Hole ◽

Area Of Interest ◽

Transmission Electron ◽

Polished Side ◽

Preparation Techniques

The use of transmission electron microscopy (TEM) to support process development of advanced microelectronic devices is often challenged by a large amount of samples submitted from wafer fabrication areas and specific-spot analysis. Improving the TEM sample preparation techniques for a fast turnaround time is critical in order to provide a timely support for customers and improve the utilization of TEM. For the specific-area sample preparation, a technique which can be easily prepared with the least amount of effort is preferred. For these reasons, we have developed several techniques which have greatly facilitated the TEM sample preparation.For specific-area analysis, the use of a copper grid with a small hole is found to be very useful. With this small-hole grid technique, TEM sample preparation can be proceeded by well-established conventional methods. The sample is first polished to the area of interest, which is then carefully positioned inside the hole. This polished side is placed against the grid by epoxy Fig. 1 is an optical image of a TEM cross-section after dimpling to light transmission.

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