扫描电镜SEM-JEOL7600F详细操作步骤
Operating procedure for JEOL 7600F High Resolution Analytical SEM
I. Specimen preparation
There are veral holders for different kinds of specimens and applications. During your initial training you should have received a general overview of the holders. Also, you should have received training on specimen mounting using the holder that best suits your specific application. Only u a holder for which you have received training by the tool instructor. If you wish to u a different holder, first contact the tool instructor.
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It is very important to know the kind of holder you are using and the way to mount specimens. For example, for the 12.5 and 26 mm holders, the correct way to mount your specimen is to flush its surface with the cylinder top face (e Fig. 1).
FIG. 1. Specimen positioning on 12.5 and 26 mm holders. (Diagram taken from JEOL’s manual.)
If your specimen needs to protrude above the cylinder’s top face (or the top face of another holder), you can still u this holder, but you need to estimate (with approx. 1 mm accuracy) the offt between the specimen and holder top surfaces. To make sure you are doing things correctly, u the sample height tool(e Fig. 2). Try to have the sample’s surface aligned with the zero offt line. If it
needs to be above this line, read the offt in the meter scale. This offt value will be ud when loading your sample in the SEM chamber.墨玉怎么鉴别真假
FIG. 2. Sample height tool. The right image shows a sample correctly flushed at the zero offt line.
II. Loading a specimen
1) Log on your ssion in the Facility Online Manager (FOM) software (icon on the desktop of
the DATA computer). After a correct login, the SEM monitor should automatically turn on.
If it does not, STOP YOUR WORK AND CONTACT A STAFF MEMBER. Never modify any physical connections or push any system buttons. Doing so is unsafe for you and the instrument.
2) Confirm that the stage is in the exchange position by checking that the EXCH POSN light on
团队建设工作总结the airlock is ON. If not:
a.Click the OFF button under Obrvation in the upper left ction of the main window
(e Fig. 3). The system diagram, located in the lower right corner of the main window, should show the beam stopped at the upper ction of the SEM column. This means that the SEM column gate is clod, if not, plea contact the tool instructor.
b.Click the Obrvation button in the upper right ction of the main window.
c.Click the Exchange Position button in the SEM Monitor window.
FIG. 3. Main window of Graphical Ur Interface (GUI).
3) Before continuing with the next step, make sure that all the stage coordinates (X, Y, R and T)
are “0.0”, except for Z, which should be “38.0”.
4) Turn on a “live” image of the chamber using the infrared (IR) camera. To do this, click on
the “Windows” key in the SEM computer keyboard and lect “IR Camera” icon.
5) Ordinarily, the airlock chamber is under high vacuum and the airlock chamber isolation valve
is open. Before loading, the lights in the airlock buttons should be: VENT-off / EVAC-on / EXCH POSN-on / HLDR-off.
6) Press the VENT button for 2 conds then relea it. (The VENT light blinks; the isolation
valve clos; N2 gas vents into the airlock.)
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海蜇王7) When the VENT light stops blinking, unlock the airlock chamber by releasing the clasp.
Open the airlock door.
8) Lock the specimen holder into the clamp on the end of the exchange rod. (The specimen
height above the top of the holder is limited to ~5 mm.) Make sure the flat side of the specimen holder lies perpendicular to the inrtion direction (e figs. 4 and 5).
FIG. 4. Locking the sample holder in place in the airlock chamber. a) Top view of specimen holder. b) and c) Identification of “flat side” with respect to dovetail channel at the ba of holder. The flat side is perpendicular to the length of the dovetail channel. d) Correct way of locking specimen holder with the holder’s flat side perpendicular to the inrtion direction. (Diagrams taken from JEOL’s manual.)
FIG. 5. Sample locked in place in the airlock chamber
IT IS VERY IMPORTANT TO CHECK THAT THERE ARE NO VERTICAL GAPS BETWEEN THE HOLDER AND THE CLIP MECHANISM. GENTLY PUSH DOWN ON THE HOLDER TO MAKE SURE IT SITS PROPERLY OVER THE CLIP.
9) Before closing the airlock chamber, check that the door’s O-ring is free of dust and dirt and
correctly positioned in the groove.
10) Clo and lock the airlock chamber and press the EVAC button. (The EVAC light blinks; the
手指工伤鉴定标准airlock is pumped to high vacuum; the isolation valve opens.)
11) Wait until the EVAC light stops blinking. Now the lights in the airlock buttons should be:
VENT-off /EVAC-on /EXCH POSN-on /HLDR-off. Also confirm that the system diagram (lower right of main window) indicates that the airlock chamber is under vacuum (gray color)陶泥作品
and that the airlock isolation valve is open.
12) Lower the specimen-exchange rod horizontally without pulling along its axis (e Fig. 6).
Once it is completely horizontal, the low pressure in the chamber may suck the rod in. This is normal, it will stop by itlf due to friction.
FIG. 6. Lowering of specimen-exchange rod. (a) Initial vertical position. (b) Detail of location of the plastic stopper.
(c) Lowering of rod without pulling along its axis. (d) Fully horizontal position. Rod is held extended due to friction in sliding metal parts. Note that plastic stopper is pushed down when rod is horizontal as shown in (e).
13) Fully inrt the specimen-exchange rod, keeping the holder horizontal, until you feel it come
to a firm stop. Look at the chamber live image to detect this event. Then apply more force to lock the holder in the SEM stage (e Fig. 7).
FIG. 7. Lo cking holder in SEM stage. (a) Inrtion of rod by pushing horizontally along rod’s axis. (b) Rod position when it first touches the SEM stage. (c) Rod position with holder locked in SEM stage.
14) After confirming that the HLDR light has lit up, fully retract the exchange rod horizontally
until the plastic stopper snaps and comes up (e Fig. 8). Let the rod sit on the stopper and then tilt up the exchange rod without pulling along its axis. Now the lights in the airlock buttons should be: VENT-off / EVAC-on / EXCH POSN-on / HLDR-on.
FIG. 8. Retracting exchange rod. (a) Fully retracted and resting on the plastic stopper. (b) Detail of rod resting on plastic stopper. C) Lifting of rod to its vertical position without using any force along rod’s axis.
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15) Click on the Specimen Offt button in the graphical ur interface (GUI) and lect from
the list the holder you installed. If your sample has an offt (in mm) measured with the sample height tool (e Fig. 2), enter it in the specimen surface offt field of the specimen holder pop-up window (e Fig. 9).
FIG. 9. Graphic ur interface showing the specimen holder popup window.
III. Obtaining an image
1) Wait until the chamber vacuum is at 5x10-4 Pa or lower. Open the Gun Isolation Valve by
clicking the ON button under Obrvation.
3) Select the SEI detector and SEM mode, and click on the working distance (WD) in the image
info area of the GUI (e Fig. 10). VERY IMPORTANT: Only click on WD when in SEM (high mag mode), never do it in LM (low mag mode). Select 15 mm from the list and click “OK” in the window that pops up after clicking WD. This action will focus the beam to
a WD of 15 mm and will bring the stage to Z=15.0+OFFSET. If the stage doesn’t move,
check that the ZFC button is “on” (green). Keep an eye on the movement in the IR camera window.
