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  LABORATORY OF SCANNING ELECTRON MICROSCOPY (L-4)

Scope of accreditation of research laboratory No AB 120
issued by Polish Centre for Accreditation Issue No. 12 of 7 July 2015.

 

Head of the laboratory

The experts

Prof. Marek Faryna, PhD, DSc, Eng.
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Agnieszka Bigos, PhD
Piotr Bobrowski, PhD, Eng.
Robert Chulist, PhD, Eng
Anna Korniewa-Surmacz, PhD, Eng.
Magdalena Miszczyk, PhD, Eng.
Anna Sypień, PhD, Eng.
Joanna Wojewoda-Budka, PhD


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

e-mail: Adres poczty elektronicznej jest chroniony przed robotami spamującymi. W przeglądarce musi być włączona obsługa JavaScript, żeby go zobaczyć. , website: http://www.imim.pl


 The Laboratory L-4 has three scanning electron microscopes to disposal

1. Dual beam high-resolution Scanning Electron Microscopy FEI Quanta 3D FEGSEM integrated with the EDAX Trident system (Apollo 40 EDS spectrometer, TEXS WDXS spectrometer and Hikari EBSD camera)


The Quanta 3D FEG is the most versatile high-resolution, low vacuum dual beam scanning electron microscope for 2D and 3D material characterization and analysis. Innovative electron and ion optics combined with unique environmental SEM operating mode expands laboratory's capabilities, providing better, faster and more comprehensive materials characterization, analysis and sample preparation.
The Quanta 3D FEG's novel field-emission electron source delivers clear and sharp electron imaging. Increased electron beam current enhances EDXS and EBSD analysis. Three imaging modes, i.e. high-vacuum, low-vacuum and ESEMTM are to disposal. Imaging and microanalysis from all specimens with or without preparation is possible. In-situ studies of the dynamic behaviour of materials at different humidity levels and temperature (up to 950oC) is also within the Quanta 3D FEG's capabilities. High current FIB enables fast material removal. Automated FIB sectioning recipes enable accurate cross-sectioning. Quanta 3D FEG features live SEM imaging while milling, making it a superior solution for fast preparation of large samples over a wide range of materials.

The Quanta 3D FEGSEM equipped with additional systems, i.e. EDXS, WDXS and EBSD enables 2D and 3D analysis of chemical composition and crystallographic orientation.

The Quanta 3D performs the following investigations:

  • Microstructure characterization including nanomaterials
  • Analysis of morphology and chemical composition of non-conductive samples in variable pressure environment
  • Analysis of orientation topography of crystalline materials with complete phase identification
  • Three-dimensional analysis of chemical composition and crystallographic orientation
  • Simultaneous EDXS and EBSD mapping collected from the same are of the sample
  • In-situ investigations of phase transitions (using GATAN heating stage).

The microscope is equipped with several detectors for electron collection:

  • high vacuum Everhart-Thornley secondary electron detector (SED)
  • secondary electron detector for environmental conditions (LVSED or GSED)
  • solid state backscatter electron detector (BSED)
  • high contrast backscatter electron detector for low voltage investigations (vCD)

The EDXS spectrometer with silicon drifted detector (SDD) with 40 mm2 of the active area and spectral resolution of 128 eV (specified for the Mn Kα) enables the detection of elements down to boron.
The WDXS spectrometer with parallel beam geometry (PBS) optimized for low electron beam current and low accelerating voltage contains a turret with five exchangeable crystals for energy range from 150 eV to 10 keV:

  • CrSc structure (energy range: 200-420 eV)
  • WSi structure (energy range: 420-1100 eV)
  • OVO structure (energy range: 1100-1700 eV)
  • PET (energy range: 1700-2400 eV)
  • LiF[200] (energy range:3300-10800 eV)

The spectral resolution below is 20 eV for the entire energy range below 10 keV with the capability to analyse particular energy ranges or the continuous scanning of the entire energy range.
The WDXS spectrometer s fully compatible with the EDXS spectrometer.

2. Scanning electron microscope FEI E-SEM XL30 equipped with energy dispersive X-ray spectrometer EDAX GEMINI 4000 dedicated to variable pressure experiments

 


Features of the microscope:

  • point resolution: 3.5 nm at 30 kV, 30 nm at 1 kV;
  • range of accelerating voltages: 200 V - 30 kV;
  • range of magnifications: 10 x - 500 000 x at WD = 10 mm;
  • range of gas pressures: 0 - 20 Torr;
  • detection of secondary electrons and backscatter electrons in COMPO and TOPO mode
 

 

Features of the EDAX EDXS Genesis 4000 spectrometer:

  • Si(Li) detector with SUTW window
  • resolution 133 eV
  • detection of all elements from B
  • electron beam control in order to acquire images, lines and maps by employing its own scanning generator
  • ZAF and PhiRoZet correction procedures


 

 

E-SEM+EDXS facility is used for quantitative and qualitative analyses in microareas of both conductive and dielectrics/organic samples.


3. Scanning electron microscope PHILIPS XL30 equipped with energy dispersive X-ray spectrometer LINK ISIS, Oxford Instrument.

Features of the microscope:

  • point resolution: 3.5 nm at 30 kV, 30 nm at 1 kV;
  • range of accelerating voltages: 200 V - 30 kV;
  • range of magnifications: 10 x - 400 000 x at WD = 10 mm;
  • detection of secondary electrons and backscatter electrons in COMPO and TOPO mode

Features of the Oxford Instruments LINK ISIS EDXS spectrometer:

  • Si(Li) detector with SUTW window
  • resolution 138 eV
  • detection of all elements from B
  • electron beam control in order to acquire images, lines and maps by employing its own scanning generator
  • ZAF and PhiRoZet correction procedures

 


Sample preparation for investigations

The L-4 laboratory performs analyses on the samples supplied by the customers who have been previously informed about conditions concerning specimen dimensions and dedicated preparation.

The size of sample should not exceed 50 mm of diameter. Thickness and weight of the sample should be limited up to 25 mm and 250 g, respectively. The EDXS analyses requires the upper and bottom surfaces of the sample to be parallel. The analysed surface for quantitative measurements should be polished as flat and scratch-free as possible and in the unetched condition so as not to alter the topography or surface chemistry.

Samples are attached by carbon conductive paint or double sided adhesive carbon tape to specially designed holders.

The ones who are interested in carrying out the experiments by use of the facilities mentioned above should contact:

The Head of the Laboratory L-4:

Prof. Marek Faryna PhD, DSc, Eng.

phone: +48 12 295 28 28

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A few examples of investigations performed in the Laboratory L-4

 


Surface of Ti screw used in implantology, SE image, mag. 50x

Starch morphology, SE image, mag. 1500x, E-SEM conditions

 

 

Surface of porous silicon, Secondary Electron Image, magnification 16.000x


Pierwiastek

%.wag.

%.at.

Al Kα

1.1

2.8

Ti Kα

17.7

25.9

Ni Kα

17.8

21.2

Cu Kα

11.7

12.9

Zr Lα

31.2

23.9

Ag Lα

20.5

13.3

Razem:

100.0

100.0


Qualitative and quantitative analysis of eutectic in the TiZrAgCuNi alloy, ZAF correction.


Examples:


Resolution Image

SE Image

BSE Image


 


 
3D IPF image of grains in ferritic Crofer 22 APU steel2D IPF map of orientations acquired from bioceramics (shell of Neotrigonia )
 
Surface of glass, BSE image, low vacuum conditions. Voids and impurities are visible. Point of X-rays microanalysis is marked by dark cross in bright circleQualitative analysis of glass purity (see left microstructure)
HAp microstructure, SE image, mag. 100 000x, low vacuum conditions
Electron backscatter diffraction from Ni monocrystal