Prepared on April 22, 2007 JEOL 2010F - STEM Alignment I. Pre-alignment conditions: 1. Perform standard upper column alignment. The specimen must be at eucentric position. 2. Insert and center the 150um C2 aperture (Largest) 3. Remove the Obj. aperture if it is in. II. Align Mode: Press the STEM button on Knob Pad ONCE. This initiates the ASID align mode. Scan coils are not active. The following conditions are now automatically set in align mode. CBD 1.9nm-9, 40kx magnification. 1. Lower magnification if you can not see any beam. Center beam by Shift X and Y. Set the Objective Focus (R1) step size to 3, increase OL by 3 clicks (DV= +12), Focus probe with C2 lens (Brightness), center spot with Bright Shifts (Shift X and Y). 2. Decrease the OL 6 clicks (DV= -12) Adjust C2 lens (Brightness) clockwise until a caustic image is just observed. Center the caustic spot with Bright Tilts. 3. Repeat steps 1 & 2 several times. Set OL to DV = 0. 4. Optional: Align Gun Tilt (DEF) using anode wobble at CBD 1.9nm-9 mode. 5. Optional: Align Gun Shift using Bright Tilts at smallest spot size and gun shift at largest spot size. 6. Optional: Return to CBD 1.9-9 mode and repeat from step one above. III. Setting the desired probe conditions Now Press the STEM button on Knob Pad a SECOND time 1. Go to FasTEM Client menuSelector, in the middle of the menu, choose Probe Condition, set to Degauss first then to the operating probe condition. You may choose spot#7 for most applications. Choose the beam current and probe size needed as shown in the table. Smallest (low current) spots use DV= -16 and CL Aperture #3, High current probes use DV= 0 and CL aperture #2. However, continue using Aperture #1 for alignment. 2. Stop the scan by pressing SPOT button (one of scan mode buttons) on the ASID (above R1) (Mag should be XXXX on small green screen, if not continue pressing SPOT). A convergent beam diffraction pattern can be seen on the florescent screen. 3. Go to FasTEM Client menuSelector, Spot size DV C2 Aperture Choose the 15cm DFI camera length 3 6 75 um (#2) from the drop down list, and roughly 4 6 75 um (#2) center the BF disk in the screen center using the Bright Shifts (not Tilts). 5 6 75 um (#2) 4. a) Choose TV-align 15cm from the 6 6 75 um (#2) camera length drop down list; b) On Gatan 7 -16 30 um (#3) TV-Bot Camera, Turn Intensifier Fully 8 -16 30 um (#3) Counter-Clockwise; 3) Raise viewing 9 -16 30 um (#3) screen (R1) 3) Turn Intensifier just slightly 10 -16 30 um (#3) clockwise until you see the BF disk on the monitor. Be very careful that you do not damage the camera. Prepared on April 22, 2007 5. Roughly center beam on monitor using projector shifts (R2). Obtain a shadow image of your sample (Ronchigram). You may have to lower the objective focus by several DV values to get a low magnification shadow image. Center an amorphous part of the sample in the center of the BF disk. Return to DV value for the chosen probe condition. 5. Adjust Z-height to obtain Gaussian focus. As the Gaussian focus is approached, the shadow image magnification will become large at the optic axis (looks like a fish eye). The magnification will change with angle in such a way that the shadow image is circularly symmetric. In this case the coma-free axis can be located accurately. It is easier to see at the low current conditions. At higher currents, make sure the video image is not saturated. 6. Carefully Center the coma-free axis in the Ronchigram at the screen center with the Projector Shifts (R2) 7. Press the Condenser Wobble button (R2). Set the AMP and FREQ to #2 settings (R2). If there is a misalignment of the beam between the Condenser and objective lenses, the Ronchigram features will translate during the condenser wobble. Use the Bright Shifts (not Bright Tilts) to center the image wobble about the coma-free axis. The pattern should oscillate in and out on the coma-free axis. Optional: This is normally very close and you may skip this step for most applications. Press the HT Wobble button and use the BRIGHT TILT control to center the image wobble about the coma-free axis. This is difficult to adjust. It may be better to start with a lower magnification (out of focus) Ronchigram and slowly work towards Gaussian focus while correcting. 8. Adjust CL stigmators (L1) if infinite magnification portion of the shadow image is not symmetric Move to an amorphous specimen area if possible. At underfocus the characteristic ring of infinite azimuthal magnification can be seen. This should already be circular but can be adjusted using the CONDENSER STIGMATOR (if using the small phosphor screen, the correct shape is slightly elliptical). Use the focus knob to pass the shadow image through focus to see the effect of astigmatism. Carefully comafree axis to the center of monitor (the spot mark) using Projector Shifts (R2). 9. Optional: If you plan to use the EDS system, you will need to use the Hard Xray Aperture (HXA - second from top). Now is a good time to insert and center the aperture about the coma-free axis. It is difficult to position HXA. First try inserting the aperture and then wiggle the insertion knob gently to find the aperture. If you cannot find the hole, try removing the C2 aperture (infinite position). Another option is to use the side-to-side motion to find one side of the HXA then turn the knob back ¾ of a turn. Use the in/out drive to find the hole. Center the HXA about the coma-free axis. At the lower STEM magnifications, you will see some vignetting caused by the HXA in the STEM image. Do not collect EDS spectra from these regions. Prepared on April 22, 2007 10. Choose correct C2 aperture. (See the table above). It is difficult to find #3 (30 um) C2 aperture. The right way to insert it is: a) first turn selector knob to #3; b) then adjust the front knob (in/out drive) counter-clockwise. Carefully Position the correct C2 aperture on the coma-free axis. 11. Choose the operating camera length from the drop down list. Choose 12cm, 15cm or 30cm for JEOL ADF STEM detector. For EELS, (skip step12) choose 3cm or 4cm and use TEI DF Detector. For bright field STEM, use 15cm, 30cm or 60cm and BF TEI detector, or use high contract objective aperture to isolate the center of the BF disk. 12. If you intend to do STM-EELS, go to optional directly. a) Insert the JEOL ADF detector (the one above screen) and b) center the coma-free axis in the center of the detector using Projector Shifts (R2). If you can not see the edge of the detector, you may have to move sample around to a thicker region; c) Press EXT (JEOL ADF) on the upper left corner of ASID; Optional: For STM-EELS, choose camera length 3cm or 4cm and use TEI DF Detector (below monitor). In the Filter Control Menu, Select “TV Camera In”. You should see a CBED pattern on TV monitor. Center the BF spot to the center of monitor using Projector Shifts (R2). Take out “TV Camera In”. Choose “TEI” on the ASID (the upper left corner button of ASID). 13) To obtain a scan image: a) Press PIC (scan mode) and set the Scan Speed to the “2” mode; b) Verify FasTEM client says “PIC” and NOT “RDC” for the image mode; c) In the DigiScan window, click Search. You should now have an image on the computer monitor. If you don’t, check: EXT or TEI detector is selected, ADF detector brightness and contrast are correct (Use the assistance of Waveform monitor (check it on DigiScan window) to obtain right brightness and contrast), there is a sample and it is not too far out of focus. When recording, make sure ASID is NOT in SR mode or in sub-area PIC mode. In both cases the magnification will not be correct. If you see scan lines in your recording image, go to the tool icon on the DigiScan window and unselect the “line Sync”. If the image quality starts to degrade - it may be contaminating. A beam shower can be done by removing the C2 aperture, spread the illumination by changing the objective focus. Use shadow image to observe illuminated area. 14) To finish, a) press TEM button on the knob pad (between R1 and R2); b) take out JEOL ADF detector (pull out first then rotate (count-clockwise)); c) take TEI detector by pressing “Retracted”; d) Change C2 aperture into #1 and center it. e) Close the scan window.