Check that the pneumatic hose is disconnected!!!! (unless your using the BSE detector, of course)

Transcription

1 JEOL 7000F BASIC OPERATING INSTRUCTIONS-Ver.-2.0 Note: This is minimal operation checklist and does not replace the other reference manuals. Read the manual for Specimen Exchange (JEOL 7000 Specimen Exchange INSTRUCTIONS) before you read this manual. We need to be very careful with some types of specimens. Please consult the staff if your specimens are (but not limited to): 1) very large, tall, or heavy, 2) dusty and powdery, 3) wet or dirty, 4) magnetic. Do not click on this icon -> which is near the vacuum gauge icon. This inserts the backscatter detector without additional warning or confirmation. If you click this while the specimen is close to the pole piece or another detector is inserted (CL, EBSD), and the detector inserts you will break the BSE detector and do major damage. Our solution has been to keep the pneumatic air line that inserts the detector disconnected most of the time. Check that the pneumatic hose is disconnected!!!! (unless your using the BSE detector, of course) James Mabon/Fumiya Watanabe Page 1 9/29/2009

2 JEOL JSM 7000F Operation Procedure 1. Verify Instrument Condition: Fig. 2 You usually see an operation window like shown above in Fig. 2. Start JEOL PC-SEM 7000 software, if not running. a. Check if HT button is dark green. If it is blue or black, the instrument is not operational, please notify staff. If it is bright green the beam is on and there is likely a sample on the stage (EBSP run either in progress or finished). b. Start IR Chamberscope; shortcut is <CNTL-ALT-I> > or running desktop Icon. c. Verify vacuum is 9.63E-005 Pa (this is lowest readout will indicate) Vacuum Gauge icon: d. Stage should be at Exchange Position (X=35mm, Y=25mm, R=0, Z=40mm, T=0). If not, -> See JEOL 7000F Specimen Exchange INSTRUCTIONS. 2. Prepare and insert sample, see JEOL 7000F Specimen Instruction (Load Lock Operation) Procedure Manual. (Don t forget to set the offset.) 3. Open the Instrument Control dialog (by clicking this button on the Tool bar): James Mabon/Fumiya Watanabe Page 2 9/29/2009

3 You may initially see the Tool Bar only as seen below (Fig. 3): Fig. 3 or the Control Window may be already open as below: a. b. Fig. 4 c. d. e. f. g. a. Set desired Accelerating Voltage Use 15 kv unless you know you want a different voltage b. Verify the OL Aperture is set to 4, along with the physical aperture on the column. (We nearly always use 4) If it is not set to 4, and/or the physical aperture is not at 4 you will need to perform the reference aperture alignment. (See the JEOL 7000F Major User Alignment Procedure). This procedure is only for more advanced users. User's authorized to change the aperture should return it to 4 and perform reference alignment when finished with their session. c. Verify Mode 3 is selected. (Other mode values are used in imaging specimens with large beam currents. This adjusts the collector voltage of the E-T detector. d. Verify Column Mode - SEM e. Pre-set desired Probe Current Select Medium 7 range initially unless you know what setting you need. f. Verify Scan Rotation OFF (Top right in the Column Dialog) g. Verify DFC OFF (Bottom right in the Column Dialog) 4. Warning: If you do not properly enter the Holder Type & Offset in the Specimen Exchange dialog the operation in the next step you could cause severe damage to the instrument by causing the sample to crash into the objective lens pole piece. Check the document on specimen transfer. Also monitor the stage motion with the IR Chamberscope <CNTL-ALT-I>. ESC key will stop stage motion. James Mabon/Fumiya Watanabe Page 3 9/29/2009

4 You may also wish to use the Stage Map Function, especially, if you are using a multiple sample holder or wish to be able to store and quickly navigate to areas of interest, go to the Stage Map and Control function, and chose Stage Map. <-Stage Map Fig. 5 Points File-> Then click the Points File button which opens a window like above right. (The Points File may already be open when you click Stage Map function.) Right click in the points text area for a menu (delete, delete all, store to file etc.) 5. Move the sample to roughly the correct Z-height. Click Z-FOCUS mode button (or Alt+Z key). You will see a window like this appear at the bottom right. Fig. 6 Notice that WD is now in yyeel lll lloow when Z-control is enabled. Chose desired distance (WD value), usually 10mm, by selecting from the pop-up dialog by clicking the WD field (lower right corner) in Fig. 6. James Mabon/Fumiya Watanabe Page 4 9/29/2009

5 A prompt will ask you if the correct Holder Type and the Offset Value are selected. If you are sure that you have set the offset correctly, click YES to the Warning Dialog. The stage will start to move up toward the Objective Lens. Note: Again, you can abort stage motion with the <ESC> key When motion is completed the Z Position indicator should read WD+OFFSET. Focus value will also now be WD selected. 6. Make sure the pressure is < 5.0E-004 Pa, preferably 9.63E-005 Pa, and the image is frozen (Freeze is lit on the knob pad), then click the HT button. Its icon color will change to bright green after you click on it. You should also hear the isolation valve open:. Fig. 7 Note, after you click the icon, there is a second or two delay before you hear the valve open. Click Freeze on the knob pad to un-blank the beam and start scanning (Freezing while cycling the valve is to protect the o-ring seal) 7. Optional: Set or read probe current using PCD, if desired. (Not necessary for most cases, but for CL, EBSD, WDS, Quantomix capsules, sometimes EDS, you usually will want to measure/set the current) 8. Locate your sample at minimum magnification (usually x25 at WD=10mm) using joystick or mouse right click (right click centers point clicked in field of view). Note: at the minimum magnification the image is quite distorted ( pin-cushion distortion) around the edge. You may have to click ACB (Auto Contrast and Brightness) to even see an image if screen is black or saturated white. Click ACB or adjust Contrast and Brightness as needed. Warning: At low magnification, do not turn the Focus Knob too quickly. There is significant response lag of the stage and a chance of your sample hitting the objective lens. Always watch the sample James Mabon/Fumiya Watanabe Page 5 9/29/2009

6 distance with the Z-control window and the IR Camera while performing Coarse Focus with Z-control. 9. Coarse Focus (while in the Z-Control mode) on the sample (large knob on control/knob panel). Progressively increase magnification and locate finer and finer features. The most ideal features have edges 360 degrees around, and are not exhibiting any charging artifacts. Remember, at this point, the focus control is still moving the stage in Z direction rather than adjusting objective lens strength, therefore, you need to monitor the IR chamberscope/camera. In general, use WD ~10 mm. Working Distances of 4 and 6 mm are only for very high magnification (i.e. resolution) and require extreme caution. Longer WD's improve depth of focus. The analytical techniques have specific working distances required. Try to Course Focus (Z-Focus) up to > 50,000 magnification (not that necessary). Do not worry if the specimen stage (i.e. the image) moves some laterally during the focus in Z-Focus mode. 10. Deselect Z-Focus mode (click the Z-Focus mode icon, then the Z- Focus window will disappear). Now the focusing is done by the Objective Lens. 11. Adjust for best Focus (now with the objective lens, but still by the same Focus knob). You may want to Zoom up on a small feature and use the Reduced Scan Window button (the third from the left on the top of the control box). You may also want to select a different scan speed/averaging by clicking Quick View/Fine View buttons (two left most buttons/switches on the top row of the control box). There are two separate speeds for each "View" button accessed by simply clicking those buttons. You may want to use a smaller window during the focusing/beam alignment/stigmator operations using either the RDC image button on the control panel/pad (3 rd from the left on top) or the Screen-Reducing button (a little left of the middle on the Tool bar). 12. Perform Fine BEAM Alignment DO NOT CLICK Align Reset IN THIS MODE! You need clearly discernable nanoscale-features for this. Sometimes dust particles work fine in absence of other features. James Mabon/Fumiya Watanabe Page 6 9/29/2009

7 a. Press Align button b. Beam Align should be selected by default c. Press HT Wobbler button (a separate pad, usually located on the left side of the table) and adjust amplitude, as needed. d. Adjust X and Y (beam align) knobs on Control Panel to eliminate image shift. You want the image to go in and out of focus, but no lateral shifting (there may be significant astigmatism, either ignore it at this time or correct it if it bothers you, see step 13) e. Press HT Wobbler button to turn off wobbler when the image shift is essentially eliminated. f. Select OBJ Stigmator on alignment panel. Adjust X, Y Stigmators and Focus for the best image. Iterate until your satisfied the image is optimized. Sometimes, due to contamination or other beam effects you need to move to fresh locations occasionally (1 frame width if suitable features are available), especially at high resolution on some samples. g. Close the alignment panel 13. Focus and Stigmation may be adjusted anytime. The multi-function X/Y knobs adjust the OL stigmators when the alignment panel is closed. I prefer the minimum frame averaging of the align mode. 14. Press Photo to record a slow scan image. When the capture is done, Load/Save/Print Image Window (Fig. 8 below) will appear. Save and Export the image to your desired folder. Make sure not to save to someone else s folder. The photo frame time is easily configured but is normally set to 80 sec. and 1280x1024 size. Another way of capturing the image is to simply hit FREEZE button and wait for the scan to complete (FREEZE button will stop blinking). When the FREEZE button stops blinking, capture is done. Click to Save and Export the image. The mode and number of frames to integrate may be easily configured. See the software reference manual. James Mabon/Fumiya Watanabe Page 7 9/29/2009

8 Fig. 8 Load/Save/Print Image Window (left) will open. Click Save and Export, and Save As Window (right) will open. Save the images to an appropriate folder. Stage Map Control is often useful in navigating the multiple specimen locations (especially multi-stub and large area holders). Stage Control is another way to move the stage. This is useful for moving specific distances or "frame by frame" for complete survey of a sample. When you are done with your session, please increase the magnification to a high value (>10,000X) and click HT icon to shut off the electron beam. Follow the Specimen Exchange (JEOL 7000 Specimen Exchange INSTRUCTIONS) to extract your specimen(s). TION TO TAKE IN AN Appendix: James Mabon/Fumiya Watanabe Page 8 9/29/2009

9 Appendix A: OPERATION Panel EMEOPERATION Panel RGE SCANNING MODE QUICK VIEW button Sets one of two faster scanning speeds. Each time you press the button, you select one of the two faster scanning speeds. FINE VIEW button Sets one of two slower scanning speeds. Each time you press the button, you select one of the two slower scanning speeds. RDC IMAGE button Pressing this button reduces the scanning image on the observation screen to one quarter of the area. > 4 times faster raster. ALIGNMENT WOBB button Used for the axis alignment of the electron optical system (Stigma Center X and Stigma Center Y). Do Not Use this for Beam Align. ALIGN button Pressing the ALIGN button opens the Alignment window. Each time you press the ALIGN button, the item to be adjusted changes sequentially, enabling you to select any desired item for adjustment. You can also select any item by clicking on it directly. STIG button (ALIGN OFF) Activates the astigmatism correction mode for OL, and lights the button lamp. If you press the STIG button when the Alignment window is opened, the Alignment window will close. X and Y knobs Used for astigmatism correction or for axis alignment of the electron optical system. When the STIG button is pressed they are used as the stigmator, and when James Mabon/Fumiya Watanabe Page 9 9/29/2009

10 the ALIGN button is pressed they are used as the control knobs for the selected item. FREEZE/ACB/PHOTO buttons FREEZE button Pressing the FREEZE button lights the button lamp and freezes* the displayed image according to the configured FREEZE setting. Instant Freeze: Pressing the FREEZE button freezes the image instantly. Freeze Frame: After the FREEZE button is pressed, the image that is being scanned is frozen as soon as it has been completely acquired. Integration: After the FREEZE button is pressed, the image is frozen as soon as it has been accumulated the number of times specified in advance. ACB (Automatic Contrast/Brightness) button When this button is pressed, the button lamp blinks, and the image is set to the contrast and brightness specified in advance. PHOTO button Pressing this button lights the button lamp and starts photography. MAGNIFICATION LOW MAG button Pressing this button lights the button lamp and sets the magnification to the lowest magnification. Pressing it once again dims the lamp and returns the magnification to the previous value. MAGNIFICATION knob Selects the image magnification. An image for the selected magnification is displayed enlarged 2.47 times on the observation display. The magnification displayed applies to the photographic recording system. FOCUS AUTO button This button performs the Auto function. (Not recommended.) FOCUS knob This knob performs focusing. IMAGE CONTRAST knob Adjusts the contrast of the screen. BRIGHTNESS knob Adjusts the brightness of the screen. James Mabon/Fumiya Watanabe Page 10 9/29/2009