Texas Tech University

Student Operating Instructions for the Hitachi S-4300 SEM

0804-2014



1.0 Precheck & Prep:

1.1 Check Log sheet to see if last user has signed out and whether there is anything abnormal mentioned in the comments.

1.2 Vacuum system: a. TMP1 and TMP2 both on acc.

b. Obj. Aperture on “Heat”.

c. Evac power on “l”.

d. Ion pump lights are on.

e. SC and SEC vacuum on.

f. SC Air lock on “Auto open” and SC/SEC switch on SEC

1.3 Gun part: HV off, filament on

1.4Display switch: on

1.5 NIR displayer (to monitor the chamber) should be on

1.6 Sample assembly

1.6.1 Coat a conductive layer onto the sample as needed. Fix specimen mounts to the height adjustable specimen holder.

1.6.2 Adjust the height of the specimen holder until the sample aligns with the mark on the height gauge.

*Consult with staff on things unusual.

2.0 SEM Operation:

2.1 Sample loading

2.1.1 Precheck the air-lock toggle switch, it should be at the "C" position.

2.1.2 Vent SEC by depressing the ‘AIR' button on the low right hand side of the column unit.

2.1.3 Slide open the SEC and screw the specimen holder firmly onto the exchange rod.

2.1.4 Close the SEC, Press the ‘EVAC' button on the column unit.

2.1.5 Wait until the S.E.C. High Vac lights up on the column unit or the red square on the bottom of the screen turn into blue, and then 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 (rotate the knob for about 10 times to make sure the exchange rod and sample holder are completely detached), remove from the chamber, and turn the air lock lever to the "C" position.

2.1.8 Setup the sample mount size on the right hand column. If it is grey, click on “go home” first, wait until the “set” button shows up.

2.2 Find an image

2.2.1 Setup the high voltage and click on.

2.2.2 Adjust the image magnification couterclockwise. Click ABC to auto adjust brightness and contrast. Use the Trackball to move the sample to the area of interest.

2.2.3 Sharpen image and adjust the brightness and contrast using the Focus, Brightness, and Contrast rotary controls.

2.3 Alignment

2.3.1 Click on the aperture option and center the aperture by click the reset button at the bottom right corner. Pull the objective aperture out to “0”position.

2.3.2 Click on the beam. Center the beam position. Then insert the objective aperture. If no beam is visible, crank up the contrast and brightness until you can observe beam light, then center the beam.

2.3.2 Click on the aperture option again, adjust the two knobs on the objective aperture on the column unit to stop the image fluctuation.

2.3.3 Click on the stigma X, adjust the X, Y knobs on the control panel to stop the image shift in any direction.

2.3.4 Click on the stigma Y, adjust the X, Y knobs on the control panel to stop the image shift in any direction.

2.3.5 Click on “off” to stop the alignment procedure.

2.4 Sharpen the image

2.4.1Shorten the working distance by changing the Z value (don't make it smaller than 5 mm! Watch the sample holder as it moves upward toward the pole piece, in case of emergency, click “stop” on the upper right corner of the screen to stop collision)

2.4.2 Focus first as good as you can, then adjust the stigmator x to the best, then the stigmator y. Each time just adjust one knob. Don't try adjusting two together, you will get lost.

2.4.3 Other options, such as switching to a smaller objective aperture, or changing to a different acc voltage. In these cases, repeat the alignment and focusing procedures.

2.5 Save images Click on the capture in the setup menu to acquire an image. As you taking images, all those images will show on the left hand panel. Save them in your own folder under D drive.

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2.6 Shutting off

Click “go home” to reset the sample holder position.

Click “ off” on the setup HV panel

Set Z position back to 15 mm, magnification counterclockwise,

Turn the air lock lever to the “O” position, insert the exchange rod and screw it in the specimen holder firmly. Pull it all the way out. Then change the air lock lever to the “C” position. Press “AIR” button to open the SEC. Take your sample out. Close the SEC and press “evac” to vacuum the SEC.

 

College of Arts and Sciences Microscopy