CMA029/1
Student Operating Instructions for the Hitachi S-4300 SEM
1.0Sample Preparation:
1.1Samples 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.
2.0Procedure
2.1SEM Operation:
2.1.1Move air-lock toggle switch to the "Close" position.
2.1.2Vent air lock by depressing the ‘AIR/EVAC’ button on the column unit.
2.1.3Slide open the air lock and screw the specimen holder firmly onto the exchange rod.
2.1.4Pump the air lock by depressing the ‘AIR/EVAC’ button on the column unit.
2.1.5Wait until the S.E.C. High Vac lights up on the column unit and turn the air lock lever to the "O" position.
2.1.6Using the exchange rod insert the specimen holder into the stage.
2.1.7Unscrew the exchange rod, remove from the chamber, and turn the air lock lever to the "C" position.
2.1.8Move air-lock toggle switch to the "Auto Open" position.
2.1.9Use the Trackball to move the sample to the area of interest.
2.1.10Adjust the image magnification using the rotary control.
2.1.11Sharpen image and adjust the brightness and contrast using the Focus, Brightness, and Contrast rotary controls.
2.1.12Using the cursor, click on the photo icon to acquire an image.
2.1.13Store the image on the hard drive using the “Save Image” command.
2.1.14The image filename used should be “(photo number).bmp” and documented in the Image File Records Book including date, brief sample description and client details.
2.1.15Images are printed using appropriate software.
CMA029/1
2.2 SEM/EDX Operation
2.2.1The working distance on the SEM should be adjusted using the stage Z control to a height of 20mm for x-ray analysis.
2.2.2Set the Beam Current to approximately 8-10 in the "Analysis" mode on the Column Setup panel.
2.2.3Select the area for analysis using the appropriate Analysis Mode control.
2.2.4Start the Spirit Software using the desktop icon.
2.2.5Using 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.
2.2.6Select 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.