Scope of accreditation of research laboratory No AB 120
issued by Polish Centre for Accreditation Issue No. 17 of 12 June 2019.

Address:

Institute of Metallurgy and Materials Science Polish Academy of Sciences

ul. Reymont 25, 30-059 Krakow

phone: (48) 12 295 28 98, fax: (48) 12 295 28 04

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Equipment of laboratory

1. Transmission Electron Microscope PHILIPS CM20 (200kV) TWIN

Technical parameters of PHILIPS CM20 TWIN
accelerating voltage	200 kV
point resolution	0.27 nm
line resolution	0.14 nm
min. sample diameter	2 nm
min. magnification	1 500
max. magnification	820 000
max. tilt of thin foil	600

Description of the transmission electron microscope:

The transmission electron microscope PHILIPS CM20 (200 kV) TWIN with the EDAX Phoenix attachment for local chemical microanalysis is intended for microstructure observations, phase analysis and local chemical analysis in metals, alloys, semiconductors, ceramic materials and composites.

The operation of the transmission electron microscope is similar to that of the optical microscope used for observation of thin sections of biological materials. The function of the light source is taken over by a 200 kV electron gun, while that of glass lenses is taken over by magnetic ones. The positioning of the sample is also different in both kinds of microscopes. In the optical instrument, it is placed directly in front of the objective lens, whereas in the electron microscope, the specimen is immersed within its magnetic field . The other lenses are analogous in both types if instruments.

Schemes of optical (LM) and transmission electron (TEM) microscopes

Electron diffraction, one of the main factors that are decisive for the contrast of images obtained in transmission electron microscope, may also provide valuable information on local phase composition, as it gives an image of elementary unit cell as well as lattice symmetry of analysed crystallite.

Substitution of a beam of light with electrons, which may interact with sample material and produce atom excitation and emission of characteristic X-ray radiation, makes it possible to determine the chemical composition of analysed (local) areas.

Transmission Electron Tecnai G2 F20	FIB-Quanta 3D

The aim of the observations is to determine characteristic parameters like dislocation density, grain and subgrain size, distribution and density of precipitates and the like. Observations by means of the dark field technique are suitable to determine the type of analysed precipitate and characterize the ordering, i.e. size and shape, of anti-phase domains. Magnification calibration is performed every 6 months, which guarantees 1 % accuracy.

The aim of this procedure is to identify phases through the analysis of electron diffraction in parallel illumination (Selected Area Diffraction technique).

It is also possible to obtain information on local orientation of an analysed microstructure and on the relationships between a precipitate and the matrix.

The calibration of camera constant is performed every 6 months, which guarantees 0.01 nm accuracy of the procedures determining a lattice spacing and unit cell.

The aim of this procedure is to determine local chemical composition with high spatial resolution. It covers thin areas (10 – 100 nm) with the diameter within the range 100 to 10 nm.

This analysis is performed by means of EDS attachment of EDAX Phoenix with (Si;Li) drifted detector with UTW window sensitive to all elements down to Boron. Chemical composition of a sample may be determined either qualitatively (all elements) or quantitatively (for elements of Z>5).

EDS system calibration is performed every 6 months, which guarantees 0.5 – 0.1 % detection limit and relative accuracy of 5 – 2 % of composition, depending on the character of spectral lines of elements found in the analyzed material.

Sample preparations

Samples for TEM observations should be prepared as discs 3 mm in diameter and 0.1 mm thick.

Persons interested in this type of investigation should contact:

 

 

 Application of transmission electron microscope with EDS attachment in investigations of new high strength AlCuMgAg alloys

 

 

A map of chemical composition with plate-like precipitates of S and W phase (with the point of analysis indicated), and its corresponding microstructure (the place, in which electron diffraction was taken is indicated)