CMA029/1
Student Operating Instructions for the Hitachi S-4300 SEM
1.0 Sample Preparation:
1.1 Samples will be prepared in a variety of ways, which are appropriate to the sample type and the
information that is required from them.
1.2 Metallic, and conductive, samples do not require any extra preparation.
1.2.1 Mount samples on stubs or use a clamp.
1.3 Non-conductive specimens:
1.3.1 Mount specimens on stubs.
1.3.2 Gold coat for high resolution work.
1.3.3 Carbon coat for analytical work.
1.4 Hydrated non-conductive specimens:
1.4.1 Consult with a member of staff to determine a suitable preparation method.
1.5 Fix specimen mounts to the height adjustable specimen holder.
1.6 Adjust the height of the specimen holder until the sample aligns with the mark on the height gauge.
2.0 Procedure
2.1 SEM Operation:
2.1.1 Move air-lock toggle switch to the "Close" position.
2.1.2 Vent air lock by depressing the „AIR/EVAC‟ button on the column unit.
2.1.3 Slide open the air lock and screw the specimen holder firmly onto the exchange rod.
2.1.4 Pump the air lock by depressing the „AIR/EVAC‟ button on the column unit.
2.1.5 Wait until the S.E.C. High Vac lights up on the column unit and turn the air lock lever to the
"O" position.
2.1.6 Using the exchange rod insert the specimen holder into the stage.
2.1.7 Unscrew the exchange rod, remove from the chamber, and turn the air lock lever to the "C"
position.
2.1.8 Move air-lock toggle switch to the "Auto Open" position.
2.1.9 Use the Trackball to move the sample to the area of interest.
2.1.10 Adjust the image magnification using the rotary control.
2.1.11 Sharpen image and adjust the brightness and contrast using the Focus, Brightness, and
Contrast rotary controls.
2.1.12 Using the cursor, click on the photo icon to acquire an image.
2.1.13 Store the image on the hard drive using the “Save Image” command.
2.1.14 The image filename used should be “(photo number).bmp” and documented in the Image File
Records Book including date, brief sample description and client details.
2.1.15 Images are printed using appropriate software.
CMA029/1
2.2 SEM/EDX Operation
2.2.1 The working distance on the SEM should be adjusted using the stage Z control to a height of
20mm for x-ray analysis.
2.2.2 Set the Beam Current to approximately 8-10 in the "Analysis" mode on the Column Setup
panel.
2.2.3 Select the area for analysis using the appropriate Analysis Mode control.
2.2.4 Start the Spirit Software using the desktop icon.
2.2.5 Using the File drop down menu, select the Preferences option. In the autoname tab select the
path or create a folder to store the spectra in, and set the Index number for the spectrum.
2.2.6 Select the analysis icon (dewer icon) to begin acquisition. The acquisition will run for the
preset time or until „Stop‟ is selected. The spectrum is then saved by clicking the disk icon
whereupon the Index number is incremented. Alternatively a new name may be assigned to the
spectrum before storage.