Scanning Electron Microscope JEOL JSM - 7600F
How to Use This Manual You will be promised to obtain successful results if you follow this step by step manual gently and carefully. In order to that, you must understand following precautions. Caution Measure height of the sample holder on your specimen correctly Locate the sample holder correctly into sample exchange chamber Be gently to the rod; do not push or pull it in a disorderly manner Understand difference between actual height (Z) and Working Distance(WD) Do not use your Power, Force and Strength, because this is the Fragile, Sensitive and Delicate instrument. Proceed every single step GENTLY and CAREFULLY Never set any magnetic specimens. Magnetic properties damage FE-SEM-J seriously. Use FE-SEM-F for magnetic specimens 1
Operational flow FE-SEM-J Observation Flow 2
3 FE-SEM-J Observation Flow Step By Step
26mm Offset 38mm 0 ~ 30mm 1. Confirm error messages appears on the screen Make sure there are no error message on the SEM user interface. 2. Mount the specimen on the sample holder The height of the specimen must not exceed the cylinder top surface!! *If your specimen protrudes above the cylinder s top surface (or the top face of another holder), you need to measure the offset between the specimen and holder top surfaces. In order to read the offset, use the scale (see Fig. 1). This offset value is necessary when loading your sample into the SEM chamber. Take a note of it. The protrude height of specimen must be less than 30mm from the Cylinder top. SEM Column Maximum height of specimen Height of sample holder 12.5mm Cylinder s top surface Fig.1. Scale for measuring the protrude height from the specimen holder. The protrude height of specimen must be less than 30 mm from the cylinder top surface. The distance between 4 cylinder s top surface and SEM column must be always 38mm, which is equal as the specimen exchange position.
5 FE-SEM-J Observation Flow Step By Step
Select an appropriate sample holder for your material. Mount material correctly on the specimen holder with carbon tape. For example, the specimen holder image below, specimen surface and cylinder s top surface must be equal; specimen surface never protrude the height of cylinder s top surface (Fig.2). In case when the specimen surface need protrude the cylinder s top surface, you must obey the height limitation of 30mm. Never mount specimen with height more than 30 mm from the cylinder top. Otherwise, you will damage the SEM column. Fig.2. Specimen positioning on 12.5 and 26 mm holders. (Diagram taken from JEOL s manual.) 6
7 FE-SEM-J Observation Flow Step By Step
3. Insert Specimen into SEM Chamber Insert Your Specimen into the Specimen Exchange Chamber (SEC) 1 Make sure the user interface is presented in the monitor (Fig.3.1) (*1). 2 The stage position must be at the Specimen Exchange Position of (X, Y, Z) = (0.0, 0.0, 38.0), R=0.0, T=0.0 (Fig.3.2.h). 3 Confirm the Specimen Exchange Chamber (SEC) must be locked (Fig.3.2.g) and the illumination of EVAC and EXCH POSN buttons below the SEC must be ON (Fig.3.2.i, j) (*2). Also, the airlock isolation valve between the SEM chamber and the SEC is an open state (Fig.3.3.e), and both areas are in the high vacuum condition. 4 Click VENT of the user interface (Fig.3.1.g-1) VENT button below the SEC starts blinking. At the same time, the airlock isolation valve between the SEM chamber and SEC is closed (Fig.3.3.k). The SEC will be in air condition after N 2 gas purge into that room; meanwhile, the SEM chamber keeps high vacuum condition (Fig.3.3.l). 5 When VENT button stop blinking, remove the clamp (Fig. 3.2.h), then, open the door of the SEC. (*1)When the user interface is not running, click SEM icon on the desktop. Then, activate SEM with guest account. Pass word is not necessary. (*2) When the lights are not illuminated, a. Click OFF button below the observation tab in the user interface (Fig.3.1.a). b. Confirm the SEM column gate is closed (Fig.3.1.d). * Please call our staff if the SEM Column Gate are not able to close. c. Click Observation button (Fig.3.1.a). d. Click Specimen Exchange button(fig.3.1.f) 8
9 FE-SEM-J Observation Flow Step By Step
a b c Airlock isolation valve Open d f e g-1 g-2 Fig.3.1. FE-SEM-J User interface h i Airlock isolation valve k l Close SEC SEM chamber Air condition High vacuum condition 10 Fig.3.2. Specimen Exchange chamber (SEC) and control panel of SEC j Fig.3.3. Vacuum condition of the SEM chamber and the SEC: (k) the airlock isolation valve, (l) the SEC is in air condition but the SEM chamber keeps high vacuum condition
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6 Mount specimen holder on the base of holder in the SEC (Fig.3.4~3.6) (*3) (*3) a. Specimen with the protrude height less than 30mm from the Cylinder top is allowed to mount. b. Make sure flat side of the specimen holder set perpendicular to the insertion direction. Caution!! The specimen holder will drop off into SEM chamber and damaged SEM if it is not mounted correctly. Thus, Gently and carefully insert the specimen holder to the base. Do not make a gap between the specimen holder and the base. m n o Flat side Fig.3.4.Specimen holder :( m) top view (a diagram from JEOL user Manual), (n) top view of the actual specimen holder, (o) side view of specimen holder, indication of flat side Flat side Attached correctly Insert direction the base of holder in the SEC Gently insert the specimen holder to the base. Keep the flat side perpendicular to the insertion direction Flat side of the specimen holder must be attached to flat side of the base Fig.3.5. Correct way of locking specimen holder with the holder s flat side perpendicular to the insertion direction. 12
13 FE-SEM-J Observation Flow Step By Step
O ring 7 Before closing the door of the SEC, Confirm whether the O ring is set to the correct position without contamination (Fig.3.6).Do not touch O ring by your bear hands. 8 Gently close the door of the SEC and lock it with the cramp (Fig.3.2.h). Click EVAC button of the user interface (Fig.3.1.g-2). EVAC button below the SEC start blinking. Do not unlock the clamp during the blinking because the airlock is pumping to the high vacuum. 9 Confirm the lights of EVAC and EXCH POSN buttons have lit up (Fig.3.2.i,j). 10 Confirm the airlock isolation valve between the SEM chamber and the SEC is an open state (Fig.3.1.e), and both areas are in the high vacuum condition. Fig. 3.6. The specimen holder that is installed correctly to the base. p q Stopper 14 Fig.3.7. The overview of the SEC with the rod: (p) the rod at the neutral position, (q) the rod stopper. The rod stopper must be in the standing state when the rod is at the neutral position.
15 FE-SEM-J Observation Flow Step By Step
Transform Specimen Holder from the SEC to the SEM Chamber 11 Gently and carefully lower the rod horizontally without pulling along its axis from the neutral position (Fig.3.7.p). Keep the rod fully horizontal position(fig.3.8) 12 Gently and carefully insert the rod by pushing horizontally along the rod s axis until you feel it come to a firm stop (Fig.3.9.1,2). Then, apply little more force to lock the holder in the SEM stage. The rod is now completely contained in the SEM chamber. (Fig.3.9.3,4). 13 After confirming that the HDLR lights has lit up (Fig.3.8.s), fully retract the rod horizontally until the rod stopper snaps and comes up (Fig.3.9.6). 14 Lifting of the rod to the neutral position without using any force along the rod s axis (Fig.3.8.r). 15 Once the Specimen holder located into the SEM stage correctly, pop-up menu of the specimen holder selection appears on the user interface(fig.3.9.5). 16 Select the specimen holder currently in use (Fig.3.9.t). Enter offset value from 0mm to 30 mm in the specimen surface offset field (Fig. 3.9.u), which was measured with the scale (Fig.1). Once the rod reach to the SEM stage, it firmly stopped(fig.3.9.2). However, you must apply little more force to lock the holder in the SEM stage. When the specimen holder is not locked correctly to the stage, pop-up menu of the specimen holder selection is not appeared (Fig.3.9). When that pop-up menu is not appeared, Make sure whether you completely insert the rod to the SEM chamber Do not push the rod forcibly when it stops at the unexpected area. There might be problem. Make sure the lights of SEC are all illuminated except VENT after the specimen is able to locate to the SEM stage correctly. s r Keep flat Fig.3.8. (r) Fully horizontal position. The rod is held extended due to friction in sliding metal parts. The rod stopper (Fig.3.7.q) is pushed down, (s) HDLR light on after the specimen holder was is set up to the SEM stage correctly. 16 When the rod reach the fully horizontal position, you may feel that the rod will be slightly drawn into the SEM chamber; although, that slight movement will stop automatically by the friction.
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1 2 3 6 The rod come to a firm stop here 4 The rod stopper snaps and come up 5 t u Fig.3.9. process to insert the rod into the SEM chamber: 1Fully horizontal position, 2the rod come to a firm stop around here, 3the rod is completely inside the SEM chamber, 4 top view of 3, 5pop-up menu of the specimen holder selection, (t) Selected specimen holder, (u) input the offset value you measured with the scale (Fig.1) 18
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4. Observe your specimen 1 Wait until the chamber vacuum is at 5x10-4 Pa or lower. Open the Gun Isolation Valve by clicking the ON button under Observation. 2 Make sure the ZFC is activated (Fig.3.10.v) (*4). If ZFC is not activated, click the ZFC icon. 3 Select High mag mode 4 Click WD(Working Distance) and select 8mm from the pull down menu (Fig.3.10.x-1) (*5) or Home Position (Fig.3.10.x-2)(*6) 5 Open the Gun Isolation Valve by clicking the ON button under Observation (Fig.3.10.w) (*4) When ZFC is activated, the stage height (Z) mechanically move to (8mm + Offset) position. As a result, image will be focused approximately WD=8mm area. (*5) Do not select WD at Low Mag mode. You have to proceed this at High Mag mod. (*6) When you click Home position, the SEM stage automatically moves to (x, y, z) = (0.0, 0.0, 8.0), R=0, T=0. Therefore, you have to make sure that you input the offset correctly; otherwise, you will seriously damage the SEM column. w z-3 z-2 z-1 v x-1 y x-2 Fig.3.10. Main window of User interface: (v) ZFC mode, (w) electron beam on / off button, (x- 1) pull down menu of WD, (x-2) Home position button, (y) Specimen Exchange button, (z-1) camera button for capturing image,(z-2) Freeze button also for capturing image,(z-3) 20 Setting tab for integration set up
21 FE-SEM-J Observation Flow Step By Step
6 Adjust focus. The image will be focused at around WD = 8mm, if the correct offset number was set up. Stigma, contrast and brightness also need to adjust. 7 Search an area of interest. The Low mag mode is suitable to observe the over view of your specimen. 8 Increase magnification little by little, if required. 9 Save image. There are three process to save images a. Click Camera button (Fig.3.10.z-1). After that, Save as dialog box appears after the image once captured. b. Click Freeze button (Fig.3.10.z-2) once. The image is frozen after scanning currently ongoing finished. Select Save as from a pull down menu of File in the main menu. c. If you prefer to capture images with integration mode, you need to set up integration before clicking CF button. You can set up it with Setting (Fig.3.10.z- 3) basic setting view/ scan tab. You are allowed to create a holder within the SEM J Datastasion only. Pick up your data from the Datastation PC in the room 009 by your pen drive. After that, delete your data from the Datastation PC. Protect your data by yourself. Keep in mind that data within the Datastation will be completely deleted without notice. Basic Condition for Observation Emmision current / LC6 / 0.5~30 kv Acceleration Voltage SEM mode Minimum magnification 500x LM mode Minimum magnification 25x (depending on the spot size) Image shift Avilable over 50.000x Axisi alignemnt Wobbler starts when beam alignement is clicked. Minimize movement of the image using X and Y knob of Stigma. Capturing image Camear CF Charging effect free mode (reduce Dwell Time) Freeze Click once /capture a image with current setting scan speed // Click twice / immediately stop scanning. Integration Setting basic setting view/scan tab check use integration. Image is captured by clicking Freeze. 22
23 FE-SEM-J Observation Flow Step By Step
5. Exchange Specimen or Finishing Observation 1 Click the OFF button under Observation tab in the user interface (Fig.3.10.w) 2 Click the Exchange Position button (see Fig.3.10.y). SEM stage will be placed to the Specimen exchange position of (Z) = 38mm. 3 Gently insert the rod into the SEM chamber and transfer the specimen holder to the specimen exchange chamber (SEC) (Fig.3.9). 1. Gently and carefully lower the rod horizontally without pulling along its axis from the neutral position(fig.3.7.p) 2. Gently but completely insert the rod into the SEM chamber. 3. Gently and carefully retract the rod until the rod pass the stopper. 4. Lifting of the rod to the neutral position without using any force along the rod s axis (Fig.3.8.r). 4 Click VENT button on the user interface (Fig.3.1). 5 After VENT button below the SEC illuminated, open the door of SEC and remove the specimen holder. 6 1. For specimen exchange, set up a new specimen and repeat 3. Insert specimen into SEM chamber, 4.Observe your specimen 2. When you finish observation, close the door of the SEC and lock it with the cramp. Then, click EVAC button (Fig.3.1). 7 You are free to go after confirming following; No error message appeared on the user interface Illumination of EVAC and EXCH POSN below the SEC are now switch on Illumination of HLDR are off, which means there are no specimen holder on the SEM stage 24