MSE 460 TEM Lab 4: Bright/Dark Field Imaging Operation

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MSE 460 TEM Lab 4: Bright/Dark Field Imaging Operation Last updated on 1/8/2018 Jinsong Wu, jinsong-wu@northwestern.edu Aims: The aim of this lab is to familiarize you with bright/dark field imaging operation. You will know the principle and methods to form and record a bright/dark field image. TEM: Hitachi 8100 TEM (EPIC) Time: 3 hours You may need the notes from labs 1 and 2. Please bring them with you. You may spend the first hour to repeat what you learned in lab 2. It includes: I. Getting familiar with TEM structure, functions and knobs II. TEM startup III. Obtain good illumination IV. Set the sample at eucentric height V. Condenser lens alignment VI. Beam tilt purity VII. Objective lens alignment (Voltage center) VIII. Image focus and astigmatism correction (Fresnel-fringe method) Bright field imaging IX. A bright field image is formed using the direct beam. An objective aperture is needed to select the direct beam and exclude the diffracted beams when an image is formed. It is situated in the back focal plane of the objective lens as shown in the figure below. 1. Find and center an interesting specimen area. 2. Make sure that the sample is at eucentric height and BRIGHT field mode is selected. 3. Focus (BRIGHTNESS) the beam to crossover and press DIFF. 4. Center the direct beam of the diffraction pattern if necessary. 5. Insert OBJECTIVE APERTURE into the beam by turning the aperture handle clockwise. Note: One of the 4 apertures should be centered. If you can not see the aperture you want to use, do not touch the aperture X and Y controls. You should keep loading other apertures till you see one aperture near the center. Then you may center this aperture and turn to next one and center it again. You repeat the procedure until you find the one you want to use. 6. Press ZOOM to see a bright field image (Now the viewing screen is conjugated to the initial image plane indicated in the figure below).

Figure: objective lens imaging, back focal plane and image plane 7. Adjust fine focus and OBJ STIG if necessary. 8. Press PHOTO when STOP is lit to lift the screen and take a image by using CCD. X. Dark field imaging A dark field (DF) image is formed using a diffracted beam or a group of adjacent diffracted beams. The objective aperture is used to select the diffracted beam by either shifting the aperture or tilting the beam. The transmitted beam is excluded in dark field imaging. Tip: It is difficult to focus a DF image. Image focus should be done in BF mode. Method 1: Shifting the OBJ aperture 1. Follow the procedure to form a BF image (IX. 1-7). 2. Focus the beam and press DIFF. 3. Take out the OBJ APERTURE and have a look at diffraction pattern. 4. Re-insert the OBJ APERTURE and position it around a diffraction beam. Question: The selected diffraction beam should not be far away from the transmitted beam, otherwise, the image quality may be poor. Why? 5. Press ZOOM to see a dark field image Question: The vacuum area is dark and sample area is bright in a DF image. Why? 6. Adjust BRIGHTNESS to open the beam so that the interesting area is homogeneously illuminated. 7. Cover the viewing window. 8. Use CCD to record a DF image (you may need a long exposure time). Method 2: Central dark-field imaging 1. Follow the procedure to form a BF Image (IX. 1-7). 2. Focus the beam and press DIFF. 3. Take out the OBJ APERTURE to see the diffraction pattern.

4. Select DARK field mode. 5. Use BEAM TILT to center a diffracted beam inside the aperture hole. 6. Insert and center the OBJ APERTURE. 7. Press Zoom and center (BRIGHTNESS CENTERING) the beam to see a dark field image. 8. Illumination (BRIGHTNESS) may be adjusted before a DF image is recorded. Tip: Bright field image can be easily obtained by pressing BRIGHT button. Image focus and OBJ astigmatism can be checked in bright field mode. Press DARK button to return to DF image. 9. Use CCD to record a DF image (you may need a long exposure time). XI. Bright field imaging under 2-beam condition The specimen is tilted to 2-beam condition and a bright field image is formed using the transmitted beam selected by a centered objective aperture. 1. Tilt the specimen so that the pattern only shows two strong beams, that is, one transmission disc and one strong diffraction disc g, as shown in the diagram. Tip: If the diffraction pattern changes a lot, the interesting area may move out of the beam, which frequently occurs when the specimen is tilted along the second tilt axis no matter whether the specimen is at eucentric height. 2. Make sure that tilts are not higher than 20 degree before you insert OBJ APERTURE. 3. Insert OBJECTIVE APERTURE (which is situated at the back focal plane as shown in the diagram below) into the beam by turning the aperture handle clockwise. Check the tilting angle or contact EPIC staff if the aperture does not go in smoothly. 4. Press ZOOM and open the beam to see a bright field image (Now the viewing screen is conjugated to the initial image plane indicated in the figure below). Tip: Because specimen is normally bent, two-beam condition can be achieved in a limited area instead of whole area. Try to correlate image contrast of different areas and imaging condition of these areas. 5. Adjust fine focus and OBJ STIG if necessary 6. Use CCD to record images.

INCIDENT BEAM OBJECT OBJ LENS OBJ APERTURE -g (weak) O +g (strong) XII. Central Dark field imaging under 2-beam condition A central dark field (DF) image is formed using a diffraction beam selected by a centered objective aperture. The electron beam has to be tilted so that the diffraction beam passes through the optical axis of objective lens. Tip: It is difficult to focus a DF image. Image focus may be done in BF mode. 1. Follow the BF imaging procedure (1-10) to form an image. 2. Focus the beam and press DIFF 3. Take out the OBJ APERTURE to see the diffraction pattern 4. Select DARK field mode 5. Use BEAM TILT to move the g weak diffraction disc to the screen center as shown in the diagram. Tip: The g weak disc will become strong when it is centered. Keep the beam centered while the beam is tilted. 6. Insert and center the OBJ APERTURE. 7. Press Zoom and center (BRIGHTNESS CENTERING) the beam to see a dark field image. 8. Illumination (BRIGHTNESS) may be adjusted before a DF image is recorded. Tip: Bright field image can be easily obtained by pressing BRIGHT button. Image focus and OBJ astigmatism can be checked in bright field mode. Press DARK button to return to DF image. Tip: If time is allowed, try to record BF/DF images using different g and compare their contrast. Some defects may disappear under certain conditions, which is useful to determine the nature of the defects. 9. Use CCD to record images

XIII. Shut down the TEM (see lab 1 and 2 notes)