eTraining Introduction

Specimen Preparation

Leica Ultracut UCT



Hitachi S-4700 FE-SEM

Hitachi FB-2000A FIB


Veeco Dim 3000 AFM

Fluorescence Microscopes



WDS X-Ray Mapping Procedure

1. Prepare Sample | 2. Start Up | 3. Select and Set Stage Positions for Sample & Standard | 4. Setting up the Analysis Parameters | 5. Calibrating Standards | 6. Shut Down

1. Prepare Sample

This is the same as for WDS Quantitative Analysis Procedure under JEOL JSM-6400 SEM, except that a standard is not always required.

1.1. If using a standard, the sample and standard should be placed in a two-position specimen holder. Keep track of which one is which. The standard should be properly positioned so that it is aligned with its paper map. VIEW
1.2. Apply carbon conductive paint over the standard ring edge and the ring holder edge. VIEW
1.3. Repeat twice for both the sample and the standard (There should be 8 drops of paint total.) Do not cover the standards or your sample with the paint! VIEW

2. Start Up

This is the same as for WDS Quantitative Analysis Procedure under JEOL JSM-6400 SEM, except that the PCD does not change.

dQant32 Icon2.1. Log onto computer and load dQant32 software. VIEW
ESP Icons2.2 Hit [E][S][P] icons in the dQant32 program (element, standard, points).    
2.3. Load the sample and start up the SEM. See Operating Procedures under JEOL JSM-6400 SEM.    
2.4. kV = 20, WD = 39, Tilt = 0.    
2.6. Turn on the picoammeter. VIEW
2.7. Push the blue PCD (Probe Current detector) button (lights up) on the control console to insert the probe current detector into the beam path. VIEW
2.8. Press the [EOS] key on SEMs keyboard to launch a menu on the right SEM screen. Set beam current to 20 nA on the picoammeter using the CL. VIEW
2.9. Set aperture (objective aperture assembly) to 1. VIEW
2.10. Set CL coarse = 7, CL fine = ~55. VIEW
2.11. Readjust CL coarse until the picoammeter reads 20 nA. When finished, turn off blue PCD button (light goes off). VIEW

3. Select and Set Stage Positions for (Sample &) Standard

This is the same as for WDS Quantitative Analysis Procedure under JEOL JSM-6400 SEM, except that the sample positions are not collected.

3.1. Crank the EDS detector to the "in" position. VIEW
3.2. In the "Standard Table: Master", locate the standards you will use. To highlight these, hold [Ctrl] and select your required standards, then release [Ctrl] and right click the mouse. Hit "Show Selected Records" to show only these selected standards in the Standard Table window. VIEW
3.3. Use your standard map to locate these standards in the SEM. (As an aid in locating the standard, from the "dSspec" window, select menu "Stage > Specimen Holder Map".) Click on the stage map graphic where you want to move, then hold [Ctrl] and left click on the mouse at the same time. VIEW
3.4. Highlight your standard name in the "Standard Table: Master". Click the "Set" button at the bottom of the table. A "Setup Standard" dialogue will appear. Click "Store".    
3.5. Set and save the stage position for standards and Benoite (MAC), or Willemite (ARL). These are the fluorescing samples needed later. Refer to the STD map. Use the EDS to ensure that the elements agree with the map. VIEW
 Spectrum Acquisition IconErasure Icon3.5.1. If in doubt about the standard's composition, choose Spirit software, click "erase", and "acquire".
 3.5.2. Adjust the beam current so EDS dead time = 45%.
 Stop Spectrum Icon3.5.3. Stop acquiring, label peaks, go back to dQant32 screen. Go to the Standard Table and highlight your standard name. Click "set" and "store". Repeat above steps until all standards positions have been updated.

4. Setting up the Analysis Parameters

This is the same as for WDS Quantitative Analysis Procedure under JEOL JSM-6400 SEM, except that the stage will not be moved.

4.1. In the dQant32 program, select the Element Table. Select menu "Tables > Add New Table" and name it.    
4.2. Select menu "Element > Open Second Window". "Element Table2: 20KV" opens. VIEW
4.3. Select "Element Table2: 20KV". Select an element by clicking in the first column. Drag that element into the "Your named Element Table". Repeat for all desired elements.    
4.4. Select the first element in "Your named Element Table". Select "Standard Table: Master" and choose the standard name for that element. Click "Copy To Ele", and the standard name will be inserted into "Your named Element Table". Repeat for all elements in "Your named Element Table".    

5. Calibrating Standards

This is the same as for WDS Quantitative Analysis Procedure under JEOL JSM-6400 SEM, except that there is no fine search and a digital image is acquired.

5.1. Go to "Your named Element Table". Select the desired element and click "Get Std". Check the OM focus and adjust with fine Z-axis control.    
5.2. Hit "CSearch" (coarse search) button. This drives the spectrometer to a within a few millimeters of the peak location and opens the Probe Current detector.    
5.3. In the peak search window you will see a representation of the counts.    
5.4. You should see a Gaussian shaped peak. If not, follow the steps in the Troubleshooting topic in JEOL JSM-6400 SEM. If that does not work, contact support staff.    
5.5. You may see error boxes appear. Hit "continue" until the error boxes go away.    
5.6. In dPict32 click Acquire, then Setup Beam Raster. VIEW
5.7. If you have a folder for image storage, specify it in the Image Folder section of the Setup Beam Raster window. If not, you will need to create one in My Computer.    
5.8. In the window that opens you also need to specify: VIEW
 5.8.1. File name
 5.8.2. Image title
 5.8.3. Magnification (displayed at the bottom of the left CRT)

5.8.4. Number of pixels (usually 500 - 1000)

NOTE: The time required for map collection depends on:

  1. The number of pixels.
  2. The dwell time.

The best maps are 500-1000 pixels and 20 sec dwell time, which may take hours to collect.

 5.8.5. Sample per pixel: 25 Sampling rate: 400
 5.8.6. Under "Signal Source" and "Tag", you should check the boxes that pertain to the spectrometers you are using. Type in the element symbol that corresponds to the spectrometer number (found in dQant32 software in "Your named Element Table"). Also, be sure the SE box is checked if you are using secondary electrons, or the BSE box is checked if you are using backscattered electrons.

6. Shut Down

6.4. Reset aperture to position 4. Adjust contrast and brightness.    
6.5. CL = 10.    
6.6. Stage home position: dSspec > Stage > Home Position.    
6.7. EDS out. VIEW
6.8. Save and close all programs. Unload specimen.    
6.9. Shut off SEM as usual. See Shut Down under JEOL JSM-6400 SEM.    


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