FE-SEM X-Ray Spectral Analysis

Prepare the Column

Column setup icon.

1. Select Analysis mode in the Column SetUp window. The working distance should be 12 mm, the default position. Column icon.


2. Set the accelerating voltage to achieve at least 2x over-voltage, usually 20 kV.


Chamber camera icon.

3. Remember to turn OFF the infrared chamber camera.


EDS in at 4.5 icon.

4. Insert the EDS detector into the chamber at 4.5 mm.


5. Focus properly and be sure to avoid cracks and contamination. Increase the magnification to 500,000 times.


Collect the Spectrum

Revolution toolbar.

The software and icons refer to the 4pi Revolution® software for Mac. Click the toolbar above for a larger view.

Revolution icon.

1. Open the Revolution software on the Macintosh computer.


Revolution New Catalog icon.

2. Select File> New Catalog. This creates a "file drawer" for all of the spectra you wish to collect for a sample or specific condition.


Revolution accelerating voltage icon.

3. Before collecting a spectrum, make sure that the Accelerating Voltage is correct.


Revolution dwell time icon.

4. Choose a Dwell Time of at least 60 seconds.


Revolution acquire start icon.

5. Select Acquire > Acquire Start or select the camera icon to begin collection. Revolution camera icon.


Revolution dead time icon.

6. Make sure the Dead Time is 25%–30%. Dead Time can be adjusted by using the Condenser Lens 1 setting in the Column SetUp menu.


7. Restart the acquisition by selecting the Clear (clr) icon. Revolution clear icon.


Open KLMs icon.

8. To manually identify elements, right-click in the spectrum area and select "Open KLMs".


X-ray spectra KLMs icon.

X-ray Spectra KLMs.


Acquire stop icon.

9. To stop spectrum acquisition, select Acquire > Acquire Stop or select the camera icon. Revolution camera icon.


10. Select Edit Manual to force the quant program to use only the elements in your spectrum.


Revolution quant icon in toolbar.

11. Select the Quant (qnt) icon to perform quantitative analysis. Revolution quant icon.


Save the Data

Spectrum rename icon.

1. To give your spectrum a name, right-click on the spectrum and select "Rename Spectrum" or select Options > Rename Spectrum from the toolbar.


Revolution export icon.

2. To retrieve your spectrum and quant data, select File > Export and choose the file format, usually JPG or TIF.


Revolution new icon.

3. Turn off quant by deselecting the icon before acquiring a new spectrum. To collect a new spectrum, select File > New. Revolution quant icon.


Temporary user files icon.

4. To add a new subdirectory, open the "temporary user files" folder on the desktop and select the asterisk-like icon. Choose New Folder and make a folder entitled with your first and last names.


New folder under asterisk.

New Folder.


Save File As icon.

5. To save your spectra, select File > Save As. Navigate to your folder by selecting Desktop > temporary user files > your name and select Save.


Spectra select icon.

6. To view all of your collected spectra, use the scroll menu at the top right of the spectrum window.


Microanalysis: X-Ray Mapping