Specific Process Knowledge/Characterization/Element analysis: Difference between revisions

From LabAdviser
Jml (talk | contribs)
No edit summary
Jmli (talk | contribs)
 
(117 intermediate revisions by 5 users not shown)
Line 1: Line 1:
You can make detailed analysis on the elemental composition and distribution in a sample with 3 instruments at Danchip. The [[Specific Process Knowledge/Characterization/SEM: Scanning Electron Microscopy/Leo|Leo SEM]] and [[Specific Process Knowledge/Characterization/SEM: Scanning Electron Microscopy/FEI|FEI SEM]] are both equipped with an X-ray detector that allows you to make elemental analysis by using the technique Energy Dispersive Analysis or EDX. The [[Specific Process Knowledge/Characterization/SIMS: Secondary Ion Mass Spectrometry|Atomika SIMS]] uses a technique called Secondary Ion Mass Spectrometry or SIMS.
'''Feedback to this page''': '''[mailto:characterization@nanolab.dtu.dk?Subject=Feed%20back%20from%20page%20http://labadviser.nanolab.dtu.dk/index.php?title=Specific_Process_Knowledge/Characterization/Element_analysis&action=edit click here]'''
<!--Checked for updates on 24/8-2021. ok/ jmli-->




The technique of extracting information from the X-rays generated in a sample that is irradiated with electrons is called energy dispersive X-ray analysis or EDX. (Other acronyms are Energy Dispersive x-ray Spectroscopy, EDS, or Electron Probe Microanalysis, EPMA). The energetic electrons create core level vacancies as they collide with sample electrons in a multiple scattering process.
= Element analysis at Nanolab =


As mentioned in section 2.2 one possible decay mechanism is the emission of X-rays. The energy of the photons is determined by the difference in energy of the shells involved. Since atomic shells are unique for every element so
The following techniques for elemental analysis are available at Nanolab.
will be the transitions between them. Thus, every element has its own charateristic X-ray spectrum that can be used to determine the elemental composition.
* EDX
* SIMS (no longer available at Nanolab, SIMS service can be provided by this company: [http://www.eag.com/secondary-ion-mass-spectrometry-sims/])
* XPS (ESCA)
In the table below the three techniques are compared
 
== Comparison of EDX, SIMS and XPS ==
 
{| border="2" cellspacing="0" cellpadding="2" align="left"
!width="100" style="background:silver; color:black" |
!width="250" style="background:silver; color:black" | SEM with [[Specific Process Knowledge/Characterization/EDX|EDX]]
!width="250" style="background:silver; color:black" | [[Specific Process Knowledge/Characterization/SIMS: Secondary Ion Mass Spectrometry#Atomika_SIMS|Atomika SIMS]]
!width="250" style="background:silver; color:black" | [[Specific Process Knowledge/Characterization/XPS|XPS]] (or ESCA)
|- valign="top"
! style="background:WhiteSmoke; color:black" width="60" | Full name
! style="background:WhiteSmoke; color:black" | Energy Dispersive X-ray Analysis
! style="background:WhiteSmoke; color:black" | Secondary Ion Mass Spectroscopy
! style="background:WhiteSmoke; color:black" | X-ray Photoelectron Spectroscopy (or Electron Spectroscopy for Chemical Analysis)
|-
! style="background:lightgrey; color:black" | Technique
| style="background:lightgrey; color:black" | The primary beam of high energy electrons used in the SEM for imaging impinges on the sample atoms and leaves them in an excited state. X-rays with a characteristic energy are generated in the relaxation process. The combination of the fine control of the primary beam offered by the SEM and the detection of the X-rays makes it possible to make point-like elemental analysis.
| style="background:lightgrey; color:black" | A beam of high energy ions (cesium or oxygen) is used for sputtering off surface atoms of the sample. The material coming off the sample in this process is analysed with a mass spectrometer.
| style="background:lightgrey; color:black" | In a process in which a monochromatic beam of X-rays irradiates the sample surface, electrons bound inside the sample are knocked free to become photoelectrons. Escaping the sample with characteristic energy, these electrons not only carry elemental information but also chemical information. Analysing them respect to energy and numbers and adding an ion gun for depth profiles provide a powerful analysis tool.
|-
! style="background:WhiteSmoke; color:black" | What elements are detected
| style="background:WhiteSmoke; color:black" | Every element heavier than boron/carbon
| style="background:WhiteSmoke; color:black" | In principle every element, however, the sensitivity
| style="background:WhiteSmoke; color:black" | Every element except hydrogen and helium.
|-
! style="background:lightgrey; color:black" | Chemical information
|style="background:lightgrey; color:black"| None
|style="background:lightgrey; color:black"| None
|style="background:lightgrey; color:black"| Chemical state information
|-
! style="background:WhiteSmoke; color:black" | Sample requirements
| style="background:WhiteSmoke; color:black" | Vacuum compatible
| style="background:WhiteSmoke; color:black" align="left"|
* UHV vacuum compatible
* The sample needs to be cut into small (app. 5*5 mm) pieces.
| style="background:WhiteSmoke; color:black" align="left"|
* UHV vacuum compatible
* Sample size max 50x50 mm, thickness max 20 mm.
|-
! style="background:lightgrey; color:black" | Spatial resolution
|style="background:lightgrey; color:black"| Very precise point-like analysis is possible with SEM electron beam.
|style="background:lightgrey; color:black"| A square with dimensions of a few hundred microns is selected for analyis with a camera
|style="background:lightgrey; color:black"| Using a magnified view from a camera, a point that covers an area down to an ellipse of 40 microns may be irradiated with photons (the default size is 400 microns)
|-
! style="background:WhiteSmoke; color:black" | Depth resolution
| style="background:WhiteSmoke; color:black" | The size of the interaction volume depends on the high voltage in the SEM and the sample density: The higher the SEM high voltage the bigger and deeper the interaction volume. The more dense the material is the smaller is the interaction volume. See section 'Spatial resolution using EDX' below.
| style="background:WhiteSmoke; color:black" | The sputtering of the surface makes it possible to perform detailed depth profiling with extremely good sensitivity and depth resolution.
| style="background:WhiteSmoke; color:black" | Very surface sensitive technique. Only photoelectrons from the top layer (a few nanometers deep) escape unscattered. By using the ion beam etch, the composition of deeper lying layers can be probed.  
|-
! style="background:lightgrey; color:black" | Detection limit
|style="background:lightgrey; color:black"| Approximately 1 % atomic weight
|style="background:lightgrey; color:black"| Down to 1 ppb for certain elements
|style="background:lightgrey; color:black"| Approximately 1 % atomic weight
|-
! style="background:WhiteSmoke; color:black" | Speed of measurement
| style="background:WhiteSmoke; color:black" | Very fast and easy
| style="background:WhiteSmoke; color:black" | Time consuming
| style="background:WhiteSmoke; color:black" | Quite fast and easy
|}

Latest revision as of 09:50, 3 February 2023

Feedback to this page: click here


Element analysis at Nanolab

The following techniques for elemental analysis are available at Nanolab.

  • EDX
  • SIMS (no longer available at Nanolab, SIMS service can be provided by this company: [1])
  • XPS (ESCA)

In the table below the three techniques are compared

Comparison of EDX, SIMS and XPS

SEM with EDX Atomika SIMS XPS (or ESCA)
Full name Energy Dispersive X-ray Analysis Secondary Ion Mass Spectroscopy X-ray Photoelectron Spectroscopy (or Electron Spectroscopy for Chemical Analysis)
Technique The primary beam of high energy electrons used in the SEM for imaging impinges on the sample atoms and leaves them in an excited state. X-rays with a characteristic energy are generated in the relaxation process. The combination of the fine control of the primary beam offered by the SEM and the detection of the X-rays makes it possible to make point-like elemental analysis. A beam of high energy ions (cesium or oxygen) is used for sputtering off surface atoms of the sample. The material coming off the sample in this process is analysed with a mass spectrometer. In a process in which a monochromatic beam of X-rays irradiates the sample surface, electrons bound inside the sample are knocked free to become photoelectrons. Escaping the sample with characteristic energy, these electrons not only carry elemental information but also chemical information. Analysing them respect to energy and numbers and adding an ion gun for depth profiles provide a powerful analysis tool.
What elements are detected Every element heavier than boron/carbon In principle every element, however, the sensitivity Every element except hydrogen and helium.
Chemical information None None Chemical state information
Sample requirements Vacuum compatible
  • UHV vacuum compatible
  • The sample needs to be cut into small (app. 5*5 mm) pieces.
  • UHV vacuum compatible
  • Sample size max 50x50 mm, thickness max 20 mm.
Spatial resolution Very precise point-like analysis is possible with SEM electron beam. A square with dimensions of a few hundred microns is selected for analyis with a camera Using a magnified view from a camera, a point that covers an area down to an ellipse of 40 microns may be irradiated with photons (the default size is 400 microns)
Depth resolution The size of the interaction volume depends on the high voltage in the SEM and the sample density: The higher the SEM high voltage the bigger and deeper the interaction volume. The more dense the material is the smaller is the interaction volume. See section 'Spatial resolution using EDX' below. The sputtering of the surface makes it possible to perform detailed depth profiling with extremely good sensitivity and depth resolution. Very surface sensitive technique. Only photoelectrons from the top layer (a few nanometers deep) escape unscattered. By using the ion beam etch, the composition of deeper lying layers can be probed.
Detection limit Approximately 1 % atomic weight Down to 1 ppb for certain elements Approximately 1 % atomic weight
Speed of measurement Very fast and easy Time consuming Quite fast and easy