FEI FIB Focused Ion Beam

Transcription

1 Operating Manual Part 1 FEI FIB Focused Ion Beam IF IN DOUBT, ASK

2 1.00 IF ANYTHING UNUSUAL HAPPENS, OR IF THERE IS ANYTHING YOU ARE UNSURE ABOUT, STOP AND CONTACT ME! DO NOT PROCEED OR ATTEMPT TO FIX THE PROBLEM YOURSELF! Chemical Safety Users are required to have passed Cornell s on-line laboratory safety training courses before they can use the FIB. Do not bring chemicals into the laboratory. Do not bring hazardous samples or materials into the lab. Contact Mick Thomas or John Grazul with any questions. This is not a storage facility - do not leave or store samples here. You must take specimens, stubs, and raw material with you when you leave. Lab-supplied chemicals are limited to a squirt bottle of isopropanol, methanol, and a can of Aero-duster. Wear safety glasses and read the MSDS s before using them. A First-Aid kit is provided but this is not a substitute for professional medical help. Fire escape routes are documented on the following page. Users failing to follow safety rules will be denied access to the lab. IF IN DOUBT, ASK IF IN DOUBT, ASK

3 1.00 In Case of Fire: Close the door behind you Leave the building First Aid Kit Fire Pull Station Fire Extinguisher Emergency Shower and Eyewash IF IN IF IN DOUBT, ASK

4 1.00 Gas Safety Nitrogen gas cylinders are to be changed by CCMR staff members only Lab Telephone If you don t have a cell phone, there is a land-line phone for your use in the corner of the NION room Campus Police: Emergency: 911 John: Illness If you feel sick, please stay at home. This will require rescheduling your session, but other people will stay healthy. IF IN IF IN DOUBT, ASK

5 2.00 Rules If ANYTHING does not even SEEM right, leave everything as is and get Mick or John DO NOT attempt to repair ANY part of the microscope. DO NOT remove panels, cables, or any part of the FIB. DO NOT add any software or hardware to any computer Flash Drives (Memory Sticks) are forbidden Data MUST be removed by burning a CD DO NOT bring food or drink into 150. Wear gloves when handling samples or shuttles. Individuals failing to follow the rules will be denied access to the instrument. IF IN IF IN DOUBT, ASK

6 2.00 Penalties Failure to follow these guidelines, unprofessional behavior or careless use of the equipment will result in loss of permission to use the FIB, in addition to repair charges, if required. Training requirements No one is permitted to use the FIB until trained by Mick Thomas. Room Access No user is permitted to unlock the door into 150 for the purpose of allowing someone else in to use the FIB. User Status Signup Room Entry Access Novice (<2 sessions) Manager M-F 8am 5pm Trained (>2 sessions) Coral Card Swipe M-F 8am 5pm Experienced (>4 sessions) Coral Card Swipe 24/7 IF IN IF IN DOUBT, ASK

7 2.00 Cancellation If you sign up and then cannot use your time, cancel your time via Coral or contact Mick at least one weekday before your scheduled time. Failing to show up Failure to show up without canceling, unless due to illness or other emergency, can result in use charges If you fail to show up within 30 minutes of your scheduled starting time the FIB becomes available to other users. Publication Acknowledgements When research is published using data from the FIB, the facility and the grant number must be acknowledged, such as: This work made use of the electron microscopy facility of the Cornell Center for Materials Research (CCMR) with support from the National Science Foundation Materials Research Science and Engineering Centers (MRSEC) program (DMR ). Data Storage Data storage and safety is NOT guaranteed! Users are responsible for their data, and must copy their data to a CD in a timely fashion. Data will be periodically erased, leaving only one years data there. IF IN IF IN DOUBT, ASK

8 2.50 About this manual (Version 1.0) This is a limited use manual intended to help new users get started on the FEI Focused Ion Beam (FIB). It provides information on basic imaging, milling, and TEM sample preparation. It is not intended to be exhaustive, and there are many principles about focused ion beam practices as well as features of this microscope that are not covered by this manual. This manual will be updated and expanded as needed.

9 3.00 How to start your FIB session Log into Coral Log on to Windows on the microscope PC Click on the FEI System Control icon. Confirm the four circles in the server window turn solid green If all the circles do not turn solid green then do not proceed contact Mick Click on Start Log on to the xtm Server Click on Determine

10 3.00 Understanding the GUI setup: Main Toolbar Electron Image Ion image Control toolbars TV image Status window Activate an image quadrant by clicking in it. The bottom bar will turn blue, indicating that window is now active.

11 3.50 How to Load a Sample Click on Navigation Button Click on Unload in the software When both lights are green lift the lid and push Unload/Release The arm should move away from the shuttle, allowing you to remove it.

12 3.50 How to Load a Sample Note that the two clamping arms must be retracted BEFORE removing the shuttle Samples must not exceed the allowable height - check height using the height gauge. They must also fit inside the volume of space as shown at left.

13 3.50 How to Load a Sample The shuttle is loaded onto the arm with the three locating balls (rubies) are in the appropriate slots on the arm (inside white circles in picture below). Gently close the lid and push Clamp/Load. When loaded the rotation should be degrees; if not enter that value as shown below. 62.4

14 3.70 How to Find Your Sample in the FIB Standard stage (at right) Enter the coordinates in the boxes for X and Y as shown at right +10, , , +10 0, , +10 0, 0 For TEM stage only: Front position: X = 0 Y = 17 Back position: X = 0 Y = -17

15 4.00 How to Turn On the Beam Select the upper left hand quadrant - this activates the electron beam option Select the voltage and current from the drop -down menus Select the Beam Control icon. Click on Beam On Un-pause the beam

16 4.20 How to Link Your Sample The FIB does not know where the sample is in reference to the polepiece (vertical position). The Z value displayed in the Navigation window will be wrong. Therefore it is critical to tell the FIB where your sample is a process called Linking. Do not adjust specimen height (Z) until you have Linked at low mag. Electron column? Sample Set the magnification to about 50X and focus the beam on the surface of your sample Increase the magnification to about 1000X and refocus Now STOP Go no further until you have clicked on the Link icon

17 4.20 How to Link Your Sample (con t) Coarse alignment Using the Z control, raise the stage to 9mm, then 7mm, then 5mm, checking after each motion that the image refocuses and the Stage motion looks normal. Ifyouseearedcirclearound the Link icon when you reach 5mm then refocus andclickonthelinkicon again.

18 4.20 How to Link Your Sample (con t) Fine alignment Find a distinct feature near the area of interest around 1000X magnification. Tilt the stage by clicking on the drop-down menu and clicking on 15 degrees. Electron column 15 degrees

19 4.20 How to Link Your Sample (con t) If the feature has moved (down, for example) then move the mouse over the TV image, click on the middle button (the wheel) and a yellow line will appear. Move the mouse in the direction necessary to move the feature to the middle of the yellow + sign on the electron image. As you do this a yellow arrow will appear showing you the direction you are going. Repeat at 45 degrees (skip 30 degrees), then finally at 52 degrees. Electron column 45 degrees Reset to 0 degrees tilt

20 5.00 How to Select Imaging Conditions Field-Free: Immersion: EDX: Use for milling and general imaging Use for higher resolution imaging. For use while collecting EDX spectra. How to Select Acquisition Type Live: Average: Integrate: Continuous imaging Uses N number of frames to form an image Takes N frames and then stops

21 6.00 How to Select Detector Type ETD: TTL: STEM: CDEM: CCD: Side mounted detector Through the Lens detector Transmission detector Channeltron Dynamic Electron Multiplier TV image

22 7.00 How to Check Beam Alignment Click on Lens Align to wobble the aperture and reduce wobble, if needed. Click on Crossover to check the beam centering and improve, if needed. Correct stigmatism with hardware controls. You are now ready for electron imaging.

23 8.00 How to Correct Astigmatism Adjust the X-stigmator and Y-stigmator so that when you go in and out of focus there is no stretching of the features Uncorrected Adjust stigmators Corrected

24 9.00 Principles of Ion Milling In the simplest of examples, start with a bulk material with a film on top Add platinum to protect the sample during milling Mill away a volume of space to reveal hidden, sub-surface features

25 9.20 How to set the ion beam conditions Ion milling can occur at any angle up to about 58 degrees. However it is tyically performed at 52 degrees, when the ion beam is at normal incidence to the sample. Click in the upper right hand quadrant the bottom bar should change from gray to blue. Set the beam current to an appropriate value for your sample, keeping it mind that it is milling your sample all the time you are focusing and stigmating. Note that there is a very large range of beam currents, with the highest over 10,000 times that of the lowest, so be careful to choose the correct value for your purpose. The higher the voltage: The sharper the image The faster the milling The more the milling surface will be amorphized The higher the current: The better the S/N The faster the milling The bigger the tails on the beam In the Application drop-down menu select Si

26 9.20 How to turn on the ion beam For general milling, make sure the stage is linked and you can tilt to 52 degrees without the feature moving more than 5 um s Electron column 52 degrees If the bar below the Source is gray, click on Wake Up. It will first turn red, then yellow, then green. When the source is green, click on Beam On. Remember that imaging with the ion beam is inherently destructive. Un-pause the beam

27 9.30 How to mill our sample Select the desired geometric pattern Draw the desired size or enter it in digitally Set the depth (Z value) Click on the Play icon To stop the milling click on the Stop icon

28 9.50 How to Deposit Platinum Choose the Patterning tab Draw a box where you want to deposit platinum. Under Gas Injection > Overview right click on Cold and a Heater option will appear.. Left click on Heater Click on white box to the left of Pt Dep to insert needle