User Manual for JSM-6400 (SEM)

(This is an informative purpose only. Do not attempt to operate the SEM without superuser permission or having a sertification)
I) INTRODUCTION II) PRE-USE CHECKS III) KEYBOARD AND ON-SCREEN MENUS
Introduction Computer Keyboard Basic Screen Electron Operating System (EOS) Menu EOS screens EOS-1 (OPTICS) EOS-2 (MODE) EOS-3 (IMAGE) MEMO Menu

IV) SYSTEM OPERATION

Sample Preparation Loading the Sample and Pumpdown (2 Airlock) Turning on the Beam Aligning the Beam Viewing the Sample Taking a Picture Turning Off the Beam

I) Introduction
The JEOL 6400 scanning electron microscope (SEM) is a high-resolution SEM. It can provide beam voltages ranging from 0.2kV to 40 kV and beam currents from 10 picoamps to 10microamps. It offers high performance and low noise at low accelerator voltages. Resolution of 10 nm is attainable, and available magnifications range from 10 X to 300,000 X. The cathode is a tungsten hair pin filament. The SEM is equipped with a two-inch airlock and a probe current detector (PCD) or Faraday cup for beam current measurements. The sample stage is computer-driven.

II) Pre-Use Checks

When not in use, the JEOL 6400 is normally left with the high voltage turned off Note that all the controls required for standard sample observation are described below. Under no circumstances should users operate any other controls without first consulting staff. This includes the entirety of the vacuum system, with the exception of the sample airlocks. Prior to using the SEM you should check that all is in order. Verify that the filament knob is turned fully counter-clockwise and that the filament meter light is on. The filament button FIL toggles the meter between filament and emission current measurement. If FIL is not lit, you are looking at the emission current and should toggle to FIL; the meter should then read ~1.0 A. If the meter light is not on, the gun pressure is not acceptable. If both FIL and the meter light are lit but there is no filament current, the SEM is not usable. Report the problem on the Comments section of the logbook AND to Murat Gre. Check that the accelerating voltage is set to 0 kV and the secondary electron

detector is off using the EOS menu (see Section 3.3).

III) Keyboard and On-screen Menus

Introduction
Most of the functions of the JEOL 6400 can be accessed though keyboard and menu operations. This includes most of the knob and button controls, with a few exceptions (e.g., the filament current knob). In addition, much of the fine-tuning required for successful imaging can only be accomplished using keyboard control. The various menus through which control takes place are displayed only on the right-hand (RH) CRT. The left-hand (LH) CRT is used primarily for viewing. A cursor is displayed on one of the two CRTs at a time; the CRT in which the cursor appears is active. The cursor can be toggled back and forth between the two CRTs by pressing the escape (ESC) key.

Computer Keyboard
The most useful keys are escape (ESC) mentioned above, BREAK, the return key, and some of the pre-defined function (PF) keys. Also useful are insert (INS), and the plus (+) and minus (-) keys. Uses of these keys will be described below.

6400 keyboard

6400 panel controls

6400 knobset

Basic Screen
The basic screen is always displayed on the LH CRT; it is also displayed on the RH CRT when the menus are hidden. This screen consists of two information lines customarily located at the bottom of the screen. When a given CRT is active (i.e. the cursor is in it) and is displaying the basic screen, its information lines can be alternately shown or hidden by pressing the BREAK key. The information displayed in the lines includes a micron bar and size, a title, the accelerating voltage, the magnification and the working distance. The pre-defined function key PF1 brings up the basic screen on the RH CRT regardless of which screen is active.

Electron Operating System (EOS) Menu

PF2 brings up the EOS menu on the RH CRT regardless of which screen is active. The EOS menu consists of three screens: EOS-1 (optics), EOS-2 (mode) and EOS-3 (image). When the RH CRT is active and EOS is displayed, pressing the 1, 2, or 3 keys will call up the corresponding screen. Most of the SEM functions required for viewing can be controlled though the EOS menu. To change a parameter, make the RH CRT active using the ESC key. If the item you want to change displays a set of possible choices (e.g. the raster scan speed), position the cursor over your choice using the arrow keys. Then press the return key to select the item. If instead the item is numeric (e.g. the accelerating voltage), position the cursor over the number and press the INS key. A white command window will appear on the RH CRT. Enter the new setting and press return to make a change. You can also increment or decrement a numeric setting by positioning the cursor over it and pressing the + or - keys.

EOS screens
The following is a brief description of the contents of the three EOS screens. Ranges are shown for numeric items when appropriate. Standard settings of the other items are indicated by asterisks. When control over an item is not needed for basic use, only the standard setting of that function is listed. Settings not needed for basic use are not listed, and should not be used without consulting staff. Settings which should not be changed without permission are indicated in the following list:

EOS-1 (OPTICS)
ACC VOLTAGE: accelerator voltage, 0 to 40 kV BIAS: bias resistor setting; default for given ACC setting shown in parentheses is recommended, 0 to 6 TILT/SHIFT: gun tilt and shift, X and Y for each: -128 to 127 CL: condenser lens; controls beam current, COARSE: 0 to 16; FINE: 0 to 255 OL: objective lens, controls focus, COARSE: 0 to 255; FINE: 0 to 1023 WD: indicates distance from plane of OL to focused point, 3 to 53 mm. STIGMA: astigmatism adjust, X and Y: -512 to 511. This should be below 100 when the image is fine-tuned. Higher readings indicate misalignment of the beam or need of column cleaning. Good patterns will not be obtainable. MAG: magnification, 10X to 300,000X INST MAG: switches to a pre-defined magnification, *OFF* SEI: CONT 0 - 255 adjusts contrast of SEI image. Bright 0 - 255 adjusts brightness of SEI image PCD: probe current detector, on this SEM, can only be operated via PCD button in one of the auxiliary panels LENS CLEAR: removes hysteresis in objective and/or condenser lenses, ALL, OL, CL OPT APERT: optimum aperture for present settings; not operated via keyboard: 2 to 4 (only a recommendation, choice is up to operator)

EOS-2 (MODE)
EOS MODE: chooses operating mode of SEM; use only SEM or SEM1: *SEM*, SEM1 SCAN MODE: chooses scan mode; PIC and LSP most useful: *PIC* (picture), RD2, RD4 (reduced scan), LSP (line scan) SPEED: selects scan rate; TV and SR are fast, others are slow: *TV*, SR, 2, 10, 20, 40 , 80, 80, 320, 640 POSITION: adjusts position of reduced and line scans, X, Y: -128 to 127, zero these before alignment or writing. SEM1 mode will disable these drives. WIDTH: adjusts width of reduced scan, X, Y: 26 to 255 IMAGE SHIFT: induces static shifts in the sample image, X, Y: -128 to 127 DSPL MODE: chooses display mode; NOR, DMG and WFM most useful; YZM should normally be off DFC: dynamic focus mode, *OFF* PHOTO SPEED: selects photo speed, 40, *80*, 80, 320, 640

EOS-3 (IMAGE)
DETECTOR: actives/deactivates secondary electron detector; USE ONLY SEI: OFF, *SEI* COLLECTOR: controls application of voltage to collector of secondary electron detector, *ON* PMT LINK: links photomultiplier tube to setting, *ON* IMS CH1: chooses image source for channel one; USE ONLY SEI: *SEI* INPUT: DIG, *ANA* POLARITY: *NOR* GAIN: *128* BRIGHT: *128* IMS CH2: see IMS CH1 MIX: when on allows mixing of CH1 and CH2 signals; when off CH1 only is displayed, *OFF*

MEMO Menu
The MEMO menu is called up by pressing the PF5 key. This menu lists ten sets of predefined operating conditions; the chosen settings for various SEM parameters are listed in the lower half of the screen. To load the selected set of operating conditions, select the title of the set in the upper half of the screen using the arrow keys. Then press "L" for load. The listed set of conditions will immediately be loaded into the SEM. NOTE: loading a set of operating conditions will result in immediate application of an accelerating voltage! DO NOT load a set unless you are ready for the listed conditions to come into effect immediately. See Section 4: System Operation below. Do not change the contents of any of the pre-defined states; they are provided for the convenience of all users.

IV) System Operation

Checklist of Procedures Follow the steps outlined below to get an image on the SEM. More information on each step is provided in the following pages. A) Sign logbook. B) Prepare your specimen for insertion into the SEM. C) Verify that the ebeam system cable is un-pluged. D) Insert the specimen into the sample chamber of the SEM. E) Perform the initial setup of all switches on the SEM console. F) Saturate the Filament. G) Adjust the Gun Shift & Tilt - resaturate if necessary. H) Adjust the contrast and brightness. I) Focus the image. J) Stigmate the image. K) Record a micrograph if desired. L) Perform microanalysis if desired. M) Shut down SEM when done. N) Remove specimen. O) Sign logbook. Sample Preparation
Samples can be most sizes or shapes as long as they can be loaded through the 2 sample exchange port. Commonly, 1 or 1.25 metallographic preparations will be examined in the SEM. Samples must be clean and dry, i.e., free from moisture, oils, grease, and particles that could the vacuum system. If the chamber becomes contaminated, the contaminants can be "ironed on" to your sample by the beam. Once this happens, it is usually impossible to remove the contaminants from your sample. Gloves must be worn when handling samples and sample holders. Note that nonconductive materials are subject to "charging" and for best results should be coated with a thin layer of gold. For cross-sections, cleave the sample through the area of interest. The sample should be as small as possible, but large enough that it can be securely held by the sample holder. If the sample is to be coated with gold, it should be coated after cleaving. For cross-sections, use the spring loaded sample holder for securing the sample. The "Z" axis knob on the stage is calculated from the sample holder top. If the sample must be secured to the holder, use SEM-compatible (vacuum compatible and conductive) carbon paint. Write Murat Gre (gure@fen.bilkent.edu.tr) if you have questions about SEM compatible adhesive. After attaching or securing your

sample to the sample holder, the sample holder is mounted into the larger dovetail holder. This dovetail holder will slide or "dovetail" over the stage in the SEM chamber. For cleaved cross-sections, it is recommended that you mount the sample so that the cleaved edge is parallel to the longer side of the dovetail holder.

Loading the Sample and Pumpdown (2 Inch Airlock)

1) The sample is loaded using a threaded rod; this rod is mounted through the center of a thick, circular viewport. The viewport allows you to visually guide the dovetail holder onto the stage and visually assess the orientation of the sample for tilt and rotation before viewing on-screen, where orientation is not as obvious. 2) Thread the screw at the end of the sample loading rod into the bottom hole of the dovetail holder, and hook the clip attached to the viewport over the screw. The clip secures the sample holder to the viewport until you are ready to move it onto the stage; if you don't use the clip, the sample and rod will move forward into the door, possibly damaging your sample or the door! If the rod does not easily slide through the viewport vacuum seal, apply grease to the rod sparingly. 3) Verify that the working distance (Z height) is set to the specimen exchange distance of 39mm; the red light on the front of the airlock exchange panel will come on to indicate that the working distance is correctly set to 39mm. Also check that the fine Z micrometer is set to 2.0 mm; it is located between the X and Y micrometers. 4) Set the stage to its home position (250 on the X and 350 on the Y travel counter). Manually adjust the rotation (angular and circular) counters to zero. Warning: Any operations on the optics table must be done gently, without disturbing the table. 5) Check the viewport and airlock o-ring for dust, remove dust to make a good seal. Hold the viewport with the sample facing towards the SEM chamber against the oring seal at the two-inch airlock entrance. Press the illuminated white button on the airlock chamber and wait for the light to go out. The light is on a timer and should allow enough time for the chamber to evacuate. Improper evacuation of the airlock can cause the vacuum system to dump when you open the airlock door resulting in down time! 6) When the light goes out, open the airlock door by rotating the airlock knob towards you 1/4 of a turn. Slide the door open by pulling the knob to the right, about 3". Be gentle. There is a clip in the airlock for this. Do not lock it with the knob as it will get debris on the door o-ring. The light in the SEM chamber should come on when you open this door. If the light is off, then the secondary electron detector is on. To turn off the detector, select OFF under DETECTOR in the EOS-3 menu (see Section 2 above). 7) Carefully push the sample rod into the chamber and slide the dovetail holder onto the stage. You may have to slightly raise the sample holder in order to get it onto the stage. The sample holder should NEVER have to be forced onto the stage. 8) Unscrew the threaded rod CCW from the dovetail sample holder. Make sure that the rod is completely unscrewed before retracting or you may pull your sample off the stage. 9) Gently retract the rod until the screw is secured in the clip attached to the viewport (you will feel a click when this happens). 10) Slide the door closed and turn the knob 1/4 turn away from you until the flat area on the knob is parallel to the floor. 11) Holding the rod near the viewport, press the white airlock button and wait for the light to go on. Make sure that you hold the rod during the venting of the airlock or the rod could fall to the floor! 12) Remove loading rod and place it in its holder. 13) Verify that the vacuum system is functioning properly. The filament meter light should still be on; this indicates the pressure is low enough to apply high voltage. If the filament light is off or there has been a significant rise in column pressure, there may be a problem in the vacuum system. Report the problem on FAULTS. If the

filament light has gone out, the SEM SHOULD NOT BE USED, AND YOU SHOULD LEAVE YOUR SAMPLE INSIDE. Contact Murat Gre to have your sample removed. 14) Never open the airlock door to the specimen chamber unless you have just pumped out the airlock. It will not preserve the vacuum and unless pumped immediately before opening, will cause the vacuum to crash, shutting down the SEM!

Turning on the Beam

There are two methods by which the beam can be started. Method 1 is presented here, that is a manual procedure. Method 2 is presented after this section and is an automated setup. Note: Method 2 is recommended for most users! Note: The area swept by the beam either on the screens or on the sample is called the raster.

Method 1
1) Bring up the information bar in the basic screen (using ESC and BREAK), or display EOS-1 in the RH CRT. Increase contrast on screens so that display information is visible. Verify that the machine is in SEI mode (SEI button will be lit). If not, press the SEI button or select SEI under IMS CH1 in EOS-3. 2) Check that the probe current detector, which collects the beam current for measurement, is not in the beam path. The blue PCD button in the auxiliary panels should be out (unlit). 3) On the JEOL keyboard, set SCAN options to FAST and single line scan (LSP) by pressing the FAST and MODE buttons (buttons will illuminate). This may also be accomplished using EOS-2. The MODE button toggles between line, cursor and point options. Continuing to press MODE will eventually bring up the line scan. Use the BRIGHTNESS and CONTRAST knobs (SEI IMAGE) to adjust the signal so that the line is positioned just above the bottom of the screen. 4) Apply an accelerating voltage. You can set the accelerating voltage by turning the ACCEL VOLTAGE knob, by changing ACC VOLTAGE in EOS-1, or by or using the MEMO menu to load a pre-defined state. 20kV is a good setting to begin with. The voltage is displayed in the information lines of the basic screen, and also in EOS-1. Note that higher voltages will give increased resolution, but also may damage your sample. After setting the desired accelerating voltage push Accelerating Voltage ON button - the button will light up. 5) Check that the objective aperture you desire is in place. One of four apertures (1, 2, 3, or 4) can be chosen. Aperture 1 is the largest and 4 the smallest. Generally 1 will be used for low voltages or high probe currents whereas 4 will be used for high voltages or low probe currents. Aperture 3 is used for most work. When you have applied an accelerator voltage and chosen a condenser lens setting, the optimum aperture will be displayed under OPT APERT in EOS-1. If you know in advance what aperture you wish to use, you can select it before applying an accelerator voltage. 6) To change from aperture 4 to 3 for instance, gently pull the aperture selection knob on the SEM column straight out. When the number 3 is visible, rotate the control toward you; it will lock in place. To change from aperture 3 to 4, simply rotate the knob away from you and it will automatically move inward. 7) Rotate FILA (filament current) knob clockwise slowly while watching both the screen. You should see the signal on the screen move upward, decrease sharply and then increase again before leveling off. This point is saturation for the tungsten filament, stop increasing the FILA knob now. NEVER INCREASE THE FILA KNOB BEYOND THIS POINT; DOING SO WILL DRASTICALLY SHORTEN THE LIFE OF THE FILAMENT. If the line scan is flat and shows no response to filament current, there are three likely culprits. The secondary electron detector may be off; the Probe Current Detector may be intercepting the beam (PCD in); or the gun tilt and shift

settings may be far off (see Section 4.4 below). You should also check the SEI brightness and contrast. The Emission Current Meter should read about 230 A 15kV with standard bias selected. If not, report this in Faults.

Method 2 Aligning the Beam

The objective of this alignment is adjust the beam so it drops straight down the column. This is accomplished by adjusting the shift and tilt at high and low beam currents respectively. 1) Ensure that the SEI button is lit and set the SCAN, MODE to LSP (a ragged line is seen on the LH CRT). To align the beam straight down the column, press the SHIFT button so that it is dimmed. The tilt/shift knobs will now change the gun tilt. Adjust the PROBE CURRENT knob clockwise; this changes the coarse condenser lens (CL COARSE) setting so as to minimize the SEI signal. Choose a high setting (e.g. 16). Equivalently, you can also use EOS-1 to set CL COARSE. Adjust the X and Y tilt/shift knobs to maximize the signal on the LH CRT. You may find it easier to find the optimal tilt and shift settings by maximizing the current detected by the probe current detector (PCD). Pressing the PCD button (RH upper panel beside CRT) inserts the probe current detector into the beam path. The beam current is then measured by Keithley picoammeter located on LH side of SEM control console. 2) Press the SHIFT button again to enable the shift feature (SHIFT button light will go on). The tilt/shift knobs will now change the gun shift. Adjust the PROBE CURRENT knob counterclockwise until you reach CL COARSE of 1 or the signal drops near to zero. This increases the probe size and is equivalent to decreasing the CL COARSE setting in EOS-2. Use the X and Y tilt/shift knobs to maximize the current. Continue to reduce the CL COARSE setting and maximize the signal with the tilt/shift knobs until you have done so at CL COARSE of 1. 3) Repeat the adjustment of gun tilt (TILT button lit) at high CL COARSE settings and gun shift (TILT button dimmed) at low CL COARSE settings until the settings remain unchanged as you go from high CL to low CL and back. Resaturate the filament as described above in TURNING ON THE BEAM.

Viewing the Sample

1) You may now adjust the working distance according to your requirements. Smaller working distances give better resolution, but if you have a large sample that needs to be tilted, consult the chart on the front of the SEM chamber for the safe working distance for your particular sample. This chart details the X, Y, and Z distances allowable for a given sample size and tilt; the black zone indicates the safe operating regions. For small samples, a working distance of 15 mm is a good operating distance. If the sample is not flush with the top of the holder, focus on the high point, read the working distance on the PNU printout or EOS. 2) On the FUNCTION keyboard, set the SCAN option to picture by pressing the PIC button. There are three PIC settings: a full screen view (PIC in EOS-2), and two smaller screen views (RD2 and RD4). Each time you press the PIC button, you will toggle to one of these three views. 3) Confirm the scan rotation is on and that the tilt correct is set to zero (fully counterclockwise). These controls are located in one of the auxiliary panels in the SEM console. The scan rotation changes the orientation of the image on the screen and is useful for aligning sample axes with the screen axes. The tilt correct compensates for the foreshortening of the image of a tilted sample by intentionally stretching the image along the X-axis. If your sample is not in fact tilted, a non-zero tilt correction setting will lead to incorrect magnification along the tilt axis. 4) Using the FUNCTION keyboard, verify that the FINE focus button is off (not

illuminated); this disables the fine focus, and allows for coarse focusing of the sample. (The fine and coarse focus are used to adjust the objective focus.) Adjust focus knob until you can see the sample holder. You can toggle between coarse and fine focus by pressing the FINE focus button. You may have to use the joystick to move the stage and sample holder directly under the beam. 5) Move your sample using the joystick to the area of interest. Optimize focus by watching the LH CRT while adjusting the fine focus. Alternatively, you can use the single line scan mode (press the MODE button) to optimize focus. At low magnifications and coarse focus, adjust the focus knob until the signal exhibits the sharpest peaks possible. At low beam current (high condenser lens settings) it may be easier to use the RH CRT to adjust the focus. This screen shows an averaged image and is quite useful when dealing with a noisy image. 6) You must make final alignment of the beam with the objective apertures. Make certain the SEM is in SEM1 mode; do so by selecting SEM1 under EOS MODE in EOS-2. SEM1 disables the image shift capability of the JEOL 6400. If you remain in SEM mode, any image shift present will interfere with the aperture alignment. In SEM mode, you may set shifts to zero, read on EOS page. 7) Find a small speck of bright material on your sample and focus on it. Make this adjustment at a magnification of 5000X or higher. Press the WOBBLE button and look at the LH CRT (not the RH CRT). The WOBBLE button automatically over- and under- focuses the SEM. Misalignment of the beam with the objective aperture will cause the image to shift from side to side (X) or up and down (Y). Adjust the X and Y aperture center- ing knobs to minimize motion of the image. The X and Y knobs are on the aperture selection control on the SEM column. The Y adjust is on the end of the con- trol, while the X adjust is comes out of its side. When you have finished, return the JEOL 6400 to full SEM mode (select SEM under SEM MODE). 8) Adjust the X and Y stigmator knobs until you get the most "real" looking image (equivalent to changing STIGMA settings in EOS-1). These knobs control the beam shape, changing it from an oval to a round shape (best image is with a round beam). You will get better results if you make this adjustment at a higher magnification (an increase of 10,000 if possible) than you plan to use for viewing or picture taking. You should make these adjustments while looking at a very small feature (about 100 nm in lateral dimensions). To adjust the position of a feature in the screen while at high magnification, it is useful to use the electrostatic image shift described above. The image position can changed with the X and Y IMAGE SHIFT knobs. To activate the image shift feature, press the POSITION button so that it is dimmed. 9) At high magnifications, adjusting the focus and stigmators may not be sufficient to bring the sample into good focus. In this case, you will need to adjust the PROBE CURRENT; this changes the beam's diameter. You will get greater resolution with a narrower beam. To narrow the beam, rotate the PROBE CURRENT knob clockwise. You should now see more detail, but you will also have more noise visible on the screen (if you take a photo, this noise should not appear on the photo). You will have to compromise between the amount of noise and the detail required. Higher accelerating voltages also give higher resolution but less surface contrast due to the greater penetration of the electron beam. Another compromise is required here. Note: If the image becomes "fuzzy" after viewing it for long periods of time, the area may be charging with electrons that are not drained away to ground. When this happens, you should move to another location for a few minutes. When you return to the area of interest if it is still not in focus, then the area has been irreversibly contaminated.

Taking a Picture
1) There are 2 screens from which you can view the image and take a picture. The left screen shows a "real-time" image while the right is an FIS (frame integrated storage) image. You can use the FREZ button on the JEOL keyboard (DISPLAY field) to

freeze the image on the right screen for taking more than one photo. 2) Press the SLOW button on the FUNCTION keyboard (SCAN field). 3) Optimize the signal contrast and brightness by pressing the WFM button on the JEOL keyboard (DISPLAY field). 5 straight, horizontal lines will appear on the left screen. Use the BRIGHTNESS and CONTRAST control knobs to adjust the scan signal so that it falls within this field during the entire scan. The height of the signal is controlled by the CONTRAST knob, while the overall position of the signal is controlled by the BRIGHTNESS knob. The highest peak of the scan signal should just hit the top line of the grid, while the lowest point should be positioned at the bottom line. Alternatively, you can try using the ACB (automatic contrast and brightness) feature to optimize the signal for picture taking, but the success of this method depends on the sample. 4) Press the WFM button again (light will go out) and the image will return to the left screen. 5) Connect the BNC cable to the Computer. Open the Image capture program and take the picture.

Turning Off the Beam

1) Load the shutdown state from the MEMO menu. This performs several functions: it returns the SEM to 0 kV without turning the accelerating voltage off; it changes the magnification to 300,000X; it turns the SEI CONT and BRIGHT down; and it changes the working distance to 39mm. There are good reasons for these settings. Leaving ACC VOLTAGE on but at 0 kV leaves some current running through the filament, keeping it clean and preheated. Turning up the magnification reduces heating of the scan coils because at high magnifications, the beam scan area is small. Turning down the SEI CONT and BRIGHT reduces the chance of accidentally burning a spot in the CRTs. Finally, setting the working distance to 39 mm leaves the SEM ready to view a just-loaded sample. 2) Press ACCEL VOLTAGE off. 3) Rotate FILA current knob fully counterclockwise. 4) Press SLOW button on JEOL keyboard (SCAN field). 5) Turn off the secondary electron detector by selecting OFF under DETECTOR in EOS-3. 6) Return to the basic screen (press PF1), hide the information bar on both CRTs (use ESC and BREAK), and put the cursor on the left screen. Turn down contrast and brightness of both CRTs. These steps are designed to prevent burn-in of images in either CRT.

Removing the Sample and Pumpdown

1) Set the stage to its home position: The X and Y at the home or center position (250 on the X and 350 on the Y travel counter). Manually adjust the tilt and rotation counters to zero. 2) Return the working distance (Z height) to the specimen exchange distance of 39mm; the red light on the front of the airlock exchange panel will come on to indicate that the working distance is correctly set to 39mm. If you have adjusted the fine Z position, return it to 2.0 mm. 3) Hold the glass viewport with the clip facing towards the SEM chamber against the oring seal at the airlock entrance. Press the illuminated white button on the airlock chamber and wait for the light to go out. The light is on a timer and should allow enough time for the airlock to evacuate. You should also visually check the o-ring for wear or contamination. If this is not the case, report the problem on FAULTS. Improper evacuation of the airlock can cause the vacuum to "dump" when you open the airlock door resulting in down time! 4) When the light goes out, open the airlock door by rotating the airlock knob towards

you 1/4 of a turn. The vacuum gauge on top of the SEM will briefly rise to the 10-2 torr range when the door is opened. Slide the door open by pulling the knob to the right. The light in the SEM chamber should come on when you open this door. If the light is not on, then the secondary electron detector is on; turn it off by selecting OFF under detector in EOS-3. 5) Carefully push the sample rod into the chamber and thread the rod into the dovetail holder on stage. Make sure that the rod is completely screwed into the holder before retracting or your sample may fall off into the chamber. 6) Gently retract the rod until the screw is secured in the clip attached to the glass viewport (you will hear a click when this happens). 7) Rotate the airlock door knob 1/4 turn toward you to unlock the door. Slide the airlock door closed and turn the knob 1/4 turn away from you until the flat area on the knob is parallel to the floor. 8) Holding the rod near the glass viewport, press the white airlock button and wait for the light to go on. Make sure that you hold the rod during the venting of the airlock. 9) Remove loading rod, unscrew the sample holder and place the rod in its holder. 10) Sign out in logbook.

Backscatter imaging
Set the BE preamplifier to SL for low to medium beam currents. On the BE IMAGE panel, set CONTRAST-COARSE to 4, CONTRAST-FINE fully CW AND BRIGHTNESS-COARSE fully CW. Select SLOW1 with the SPEED-SLOW button (or SCAN SPEED 2 in EOS-2 MODE). Set the MAGNIFICATION to a low value and press IMAGE SELECTOR-COMPO button for compositional images. Adjust the BE IMAGE, BRIGHTNESS-FINE-COMPO knob until an image appears on the CRT. Increase the probe current (using PROBE CURRENT knob) if the image is still too dark. Use the procedures previously described for SEI imaging to focus and stigmate the image. The waveform monitor (WFM) may be used to produce a useful Polaroid micrograph. Adjust BE IMAGE, BRIGHTNESS-FINE or COARSE to obtain optimum image conditions. NOTES. Higher beam currents are required at low voltages to produce usable images. Cancel COMPO by pressing IMAGE SELECTOR, SEI button.