Operating Procedure1,2,3 for the Helios NanoLab 650 SEM ...1 FEI Helios NanoLab 600 SEM/FIB Basic...

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Operating Procedure1,2,3 for the Helios NanoLab 650 SEM/FIB System

Center for Soft Materials (CSM) facilities, version 1.1 (Apr 17, 2014)

Need help? FEI Helios NanoLab 650 / 600i User Operation Manual: detailed & in-depth explanation Michael Wang: [email protected] Xin Zhang: 778-235-2650, [email protected] Abel Gebresellasie (local SFR technical support): 604-377-3644

User guidelines:

1. The Helios NanoLab 650 Dual Beam SEM/FIB system is a complex tool with various functions that are not necessarily compatible under a given experimental condition. Not all the functions can be demonstrated in one scheduled training session. Users qualified to work on the tool are unnecessarily qualified for all the functions. Therefore, users are NOT allowed to try functions that have not been demonstrated. Expert users are allowed to try challenging tasks on the tool in the presence of and with the permission of the tool owner, in order to maximize the tool capabilities.

2. Users are NOT allowed to save any data on the Helios Control computer or EDAX computer. During each tool session, all data must be temporarily saved on the Helios Support computer. Users are required to copy their data to their own storage devices and remove the data from the Helios support computer immediately after each tool session. We are not responsible for the confidentiality and security of users’ data. We supply writable CDs and DVDs for reasonable prices if users forget to bring their own storage devices.

3. Wet samples or outgas samples are NOT allowed in the Helios chamber. Any samples that might have magnetic properties, or non-conducting dry powders, should be brought to the attention of the tool owner before they can be loaded into the chamber. NEVER image magnetic samples with the Immersion (Lens) Mode.

4. If FIB application (52°) or higher tilt angle is needed, please limit your sample sizes (suggested X and Y dimensions are below 12 mm, and Z below 10 mm). Larger samples at a high tilt angle could hit the pole piece. Do NOT risk if you are in doubt. Please ask the tool owner for help.

5. Cryo SEM/FIB experiments must be scheduled with the tool owner at least one week in advance. The minimum machine time is 8 hours, which can be shared between users. SEM/FIB of non-cryo samples is unavailable during cryo experiments.

6. Data processing on the Helios Control, Support, and EDAX computers will be charged at the full amount of user fees and the time must be reserved in advance.

7. Users must remove their samples from the Nanoimaging facilities after each tool session. Users are NOT allowed to dispose hazardous sample waste within Nanoimaging facilities.

8. Users who haven’t used the Helios system for 3 months or more need to be re-trained to gain access to the tool again.

ALWAYS wear gloves when handling ANYTHING to be introduced in the vacuum system, or working with the chamber and sample stage.

ALWAYS exercise extra care when working on and around the stage to avoid contamination or damage.

ALWAYS secure samples on the holder and stage to minimize sample vibration and drift.

1 FEI Helios NanoLab 600 SEM/FIB Basic Operation Procedure by K. Song, 2008 2 UC Davis FEI 430 NanoSEM Operating Procedure by A. Gusman, 2010 3 Helios NanoLab 650 / 600i User Operation Manual, 1st Edition, FEI Company, 2012

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ALWAYS make sure sample Z is unlinked from Working Distance and move Z (downward) to zero after opening the chamber door.

ALWAYS use the “elephant” height gauge to check that the highest point of your samples is well below the MAX mark of the height gauge.

ALWAYS make sure the anti-contamination cold finger is moved out of the way during sample loading if high tilt angle of large samples is needed.

ALWAYS watch the live view of the chamber CCD camera when moving the stage.

ALWAYS re-link sample Z to Working Distance after moving the sample at millimeter steps.

ALWAYS double-check the EDAX detector is retracted out when doing FIB work, cryo evaporation, or plasma cleaning to avoid detector contamination.

ALWAYS before venting the chamber,

1. Make sure the EDAX cooling is off;

2. Make sure the GIS (Pt dep and SCE) needles and EasyLift probe are retracted;

3. Make sure the GIS heating is off;

4. Make sure the stage tilt is zero;

5. Make sure the working distance is 4 mm or larger (sample surface below the 4 mm bar);

6. Make sure both the electron and ion beams are off.

7. Make sure the Stage is unlocked

ALWAYS make sure that the chamber has been pumped down to high vacuum before leaving the tool.

NEVER bring any liquids/solvents to Nanoimaging facilities without permission of the tool owner.

NEVER attempt to start the tool if there is obviously something wrong with the tool, e.g. chamber is left vented for an unclear reason, or “Cooling water error” shows up.

NEVER vent the chamber when cryo SEM/FIB setup is in use.

NEVER force to open the chamber before it is fully vented.

NEVER touch any part in the chamber and stage with your bare hands

NEVER over-tighten when adjusting sample stage support or mounting SEM stubs on the support.

NEVER put wet samples or loose powders in the system.

NEVER put materials that will outgas in the system, e.g. un-baked polymer/photoresist films, solvents, liquids, or oils.

NEVER image magnetic samples with the Immersion (Lens) mode.

NEVER use the retractable STEM and CBS detectors without discussion with the tool owner before each tool session.

NEVER insert the GIS needle or EasyLift probe with a working distance smaller than 4 mm or with a surface having >10 µm tall outstanding features.

NEVER link sample Z to Working Distance when the stage is tilted.

NEVER tilt the stage with a working distance smaller than 4 mm.

NEVER vent the chamber with a working distance smaller than 4 mm.

NEVER leave samples unattended.

Key aspects of SEM imaging:

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1. Good vacuum.

2. Link Z to working distance without stage tilt.

3. Sufficient clearance between the samples and pole piece.

4. Select suitable high voltage and beam current to minimize charging effect and sample drift. Sometimes, suitable conductive coating (e.g. Au) is needed to for low conductivity samples.

5. Focus and stigmation correction.

6. Zero the stage tilt and switch beams off before venting.

Key aspects of SEM/FIB

1. Good vacuum, also I-bottom vacuum should be in between the I-source and Chamber vacuum.

2. Eucentric height.

3. Check Eucentric height after moving the stage.

4. Only use GIS needles and/or EasyLift probe after Eucentric height is confirmed.

5. Retract GIS needles and/or EasyLift probe immediately after use.

6. Minimize damage by ion beam imaging.

7. Think ahead.

8. Zero the stage tilt and switch beams off before venting.

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A. Tool layout

Data transfer is only allowed through the Support PC.

Support PC EDAX PC Control PC

Operate/Standby Switch

EDAX PC monitor for EDS measurements

Support PC monitor for data transfer and Internet

Control PC monitor 1 Control PC monitor 2 for large Image view

SEM/FIB chamber door

Cryo control

Liquid N2 dewar

EDAX detector

EasyLift probe

Ion source

Sample prepara

tion

e-beam quadrant

Ion beam quadrant

Navigation quadrant

Chamber view quadrant

SEM control panel

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B. Checklist:

1. The last one leaving the Helios room should turn off the room light.

2. Green light (Operate) on the system front panel should be on.

3. On the Helios Control computer (the lower right monitor), both the xT microscope Server and User Interface (UI) are running.

If you only see the UI, the xT microscope Server is minimized onto the Windows taskbar and you don’t need to worry about it.

When you only see the tiny view of the xT microscope Server, click on the Show UI button (when available) to bring up the UI.

4. Check the SEM status.

Users have to log on the UI with their assigned user name and password, if the xTm: Log on dialogue is displayed. Read “Log on the UI as a different user” for more details.

No unresolved errors in the xTm: Application Status message window in the Chamber view quadrant. This window can be brought up by selecting Tools > Application Status… if not auto-displayed. The following is an example of temporary cooling water interruptions, which were soon corrected, indicating that the tool is ok to use. Click Hide to bring the CCD camera live view to the front.

There is sufficient clearance between the stage (no tilt) and pole piece. There are no samples kept on the stage, and no needle/probe left un-retracted.

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High Voltage (HV) for both e-beam and I-beam is switched off (i.e. Beam On button is grey).

The orbital icon means the e-beam and the cluster icon means the ion beam.

Click on the e-beam quadrant and check under the Beam Control tab .

Click on the ion-beam quadrant and check under the Beam Control tab .

Chamber pressure is <4x10-6 Torr after overnight pumping (ok to use when < 4x10-5 Torr).

If chamber pressure is not displayed, park the cursor on the green microscope icon to find out.

5. Check in the logbook to make sure there is no other unresolved error from previous users.

6. Record any uncommon observations in the logbook and decide if it is safe to start your tool session.

7. Starting logging in the logbook (e.g. Date; Name; Time In) if everything is fine.

8. Samples are secured on the sample holder stub.

Ion beam HV on

Ion source ready

Ion beam HV off

Ion source ready

Ion beam HV off

Ion source not ready

e-beam HV on e-beam HV off

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C. (Optional) Logging in Windows as a different user

Note: this is only necessary if a user has requested for setting up a special Windows account.

1. The Helios Control PC and Support PC are logged in as general_user/helios when not in use.

2. Click on the Stop UI button on the tiny view of the xT microscope Server to stop the User Interface.

3. When the Hide UI button changes into Start UI, click on the Stop button to stop the xT microscope Server.

4. Wait for the server to be fully stopped and the Microscope Start button becomes available.

Right-click on the xT microscope Server tiny view bar to bring up a menu. Select/uncheck Show Tiny View in the menu to switch the xT microscope Server from tiny view to full view.

Once the server is fully stopped, all communication list items in the Advanced >> Administration view become grey (stopped), and the Microscope Start button becomes available.

5. Log off Windows (exit the general_user/helios account).

6. Log on Windows with your assigned account (or general_user/helios) and wait for a couple of minutes for the Windows to load files successfully. The xT microscope Server will automatically start.

7. Make sure the indicators for Console devices, Motion NODE1, and Imaging are all green (initialized) in the xT microscope Server. Then click on the Start button to start both the server and UI.

Watch all communication list items in the Advanced >> Administration view become green (initialized) eventually. And the UI will then start automatically.

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8. Once the UI shows up, switch the xT microscope Server to its tiny view mode.

If the xT microscope Server is not visible, minimize the UI.

Right-click on the top blue section of the xT microscope Server full view to bring up a menu. Select/check Show Tiny View to switch the server to the tiny view mode.

9. Try moving the cursor from the Control computer to the Support computer. If unsuccessful, Synergy, the keyboard/mouse sharing software, is not running properly.

If the Desktop and tool bar are not visible, minimize the UI.

Double-click on the Desktop

or click on the Windows tool bar to launch Synergy.

In the Synergy interface, click on the Apply button start sharing keyboard/mouse between the computers, and then click on the

button to close the Synergy interface.

The keyboard/mouse sharing should be effective in a few seconds.

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D. Logging in the UI as a different user

1. On the Helios Control PC, the previous user should have logged out the UI. If not, select File > Log out … and log back on the UI with your assigned username and password.

The Helios Control, Support, and EDAX PCs share one keyboard and one mouse. The cursor might be left on the EDAX or Support PC sometimes. Simply move it to right and further down, it will show up on the Control PC.

2. The xTm: Application Status message window might pop up in the Chamber view quadrant. Click Hide in the message window to bring the CCD camera live view to the front.

3. Make sure the Chamber view quadrant is un-paused.

in a quadrant indicates the quadrant is paused.

Press F6 or click the button to pause/un-pause.

If the UI is not in the quadrant mode, press F5 to bring it back.

4. Make sure there is enough clearance between the pole piece and stage.

If you see something unusual, e.g. a tilting stage, an unfamiliar stage support, inserted retractable detector, or inserted EasyLift probe or GIS needle, you might have to seek for help before any further action.

5. Upon logging on the UI, you might be asked to home the stage. This indicates that the UI has lost communication with the microscope Stage.

6. If not safe, or in doubt, skip Home Stage by clicking Cancel, and look for help.

Warning: all retractable parts must be retracted and the anti-contamination cold finger should not be in close proximity to the pole piece before performing Home Stage.

Warning: when a large sample is in place, collision might occur during Home Stage.

Warning: if a cyro stage support is in place, do NOT Home Stage to avoid breaking the liquid N2 circulating lines.

If needed, users should perform Home Stage after venting the chamber and moving the stage away from the pole piece by opening the chamber door.

If it is safe to perform Home Stage, click Ok and watch the CCD live view of the chamber.

Look for help

if this is left

by the user

before you.

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E. Unloading/loading samples

1. Make sure EDAX detector cooling is off.

If the EDAX cooling indicator is in red, the cooling is off.

On the EDAX PC, if TEAM is running, the sign indicates the cooling is off. Ok to Vent under Detector Status should be in green.

2. Make sure the GIS needles are retracted and the GIS heaters are off.

The GIS control is under the Patterning tab . Right-click on a GIS system to bring up a menu for switching the heater on/off. A ticked box indicates the needle is inserted.

3. Make sure the Easylift probe is retracted. The EasyLift control panel is under the Navigation tab .

Needles retracted, heaters off

EasyLift probe is inserted

EasyLift probe is retracted

Pt dep heater on but needle retracted Pt dep heater on and needle inserted

EDAX cooling indicator

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4. Make sure stage tilt is zero (check under the Navigation tab ), and the clearance between the pole piece and stage should be 4 mm or more (in the Chamber view quadrant).

5. Make sure the stage bias is switched off, i.e. the On button is not yellow.

Beam Deceleration control is under the Beam Control tab .

6. Make sure the High Voltage is off for both electron and ion beams, i.e. the Beam On button is not

yellow, and the stage is unlocked (lower right corner of the UI).


Click on the ion beam quadrant and check under the Beam Control tab .

A quick checklist before venting:

i. The EDAX cooling is off;

ii. The GIS (Pt dep and SCE) needles and EasyLift probe are retracted;

iii. The GIS heating is off;

iv. The Stage tilt is zero;

v. Clearance between the pole piece and sample is 4 mm or more;

vi. Both the electron and ion beams are off;

vii. The stage is unlocked.

7. Click on the Vent button to vent the chamber. Click Yes on the xTm: Vacuum message dialog.

Stage unlocked

Ion beam HV off

Ion source ready

Ion beam HV off


e-beam HV off

Stage Bias unavailable Stage Bias off

Zero tilt

Sample surface is below the 4 mm bar

Clearance 4 mm

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Vent and then Yes

8. After 2-3 minutes of venting, the chamber will hiss loudly. When the hissing sound stops and the chamber icon (lower right corner of the UI) turns grey, the chamber door is ready to open.

chamber is vented.

9. Click on the Chamber view quadrant, and go to Window > Large Image Window to bring up the full screen CCD live view in Control PC monitor 2.

10. Open the Chamber door gently while watching the CCD live view of the Chamber.

11. Lower the stage.

If Home Stage is needed, perform Home Stage when the door is fully opened.

If Home stage is not desired, type “0” in Stage > Coordinates > X, Y, and Z under the

Navigation tab , and click on the Go To button to set the stage to its lowest and centred (Ctrl+0) position.

12. Put on gloves! Carefully place the SEM stub with sample(s) in the mounting hole on the stage support and gently tighten the stub locking screw. For thick samples, the stage support should be adjusted to a lower position by loosening the support locking collars.

Never manually move any stage axis!

13. Use the sample height gauge to make sure there is enough clearance above the sample, i.e. the highest point of all mounted samples should be below the MAX mark of the gauge.

Stub locking screw driver

12 mm SEM stub tweezers

Sample height gauge

Cryo stage screw driver

SEM stub locking screws

SEM stub mounting holes

Stage support

Support locking collars

Make sure it is a red upward arrow here to move stage down to 0

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Sample surface need to be above 4 mm mark if eucentric height is needed for FIB applications.

14. Close the chamber door gently while watching the CCD live view to see how the samples approach the underneath of the pole piece.

15. Click on the Pump button to pump the chamber without sample cleaning. Push the chamber door gently at the beginning of pumping until the gap between the door and chamber is obviously reduced.

If sample cleaning is desired, click on the Pump dropdown list to select Pump with Sample Cleaning, to start chamber pumping with 5 minutes of plasma cleaning (filtered air).

.

If Pump with Sample Cleaning… is selected, following messages will appear.

16. When the chamber is pumped out, the chamber icon (lower right corner of UI) will turn green. Wait for the chamber pressure to be < 4x10-5 Torr. You are now ready to turn on the high voltage.

Chamber vacuum ready icon . For FIB applications, I-Bottom pressure must be in between the I-Source and Chamber pressure.

17. (Optional) Go to Stage > Take a Nav-Cam Photo… to obtain a photo of the sample layout when multiple samples (or a large sample) are loaded.

The Nav-Cam photo allows a user to easily move to an area of interest across a large distance by a double-click.

Green cross indicates the area of interest that is currently viewed by the electron beam.

Ok to use FIB. Look for help if FIB quality is concerned

Good for FIB applications

MAX mark Sample surface

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The Navigation quadrant: Nav-Cam Photo

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F. Linking sample Z to working distance (WD)

Warning: NEVER move the (yellow) 4 mm WD bar indicator in the Chamber view quadrant.

1. Click on the e-beam quadrant to bring up e-beam control under the Beam Control tab , indicated

by the orbital icon .

2. Once the Chamber vacuum is ready, i.e. <4x10-5 Torr, turn on the High Voltage by clicking on the Beam On button. You can select various values in the Beam Current and High Voltage dropdown lists.

3. Click on the e-beam quadrant and un-pause to bring the quadrant to live.

If the display is not in the quadrant mode, press F5 to bring it back.

Press F6 or click on the live/pause button to pause or un-pause

4. Focus the image.

Focus can be achieved by right click-holding the mouse and moving it left and right, or by

using the fine and coarse focus knobs on the SEM control panel, or using the AutoFocus function if sample has sharp features.

You might need to adjust the image contrast and brightness, by turning the contrast and brightness knobs on the SEM control panel, or moving the contrast and brightness sliders

under Detectors on the UI left panel, or using the AutoCB function if sample has sharp features.

5. Once you achieve reasonable focus, click on the Link sample Z to Working Distance button .

4mm WD bar indicator 4 mm

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Before linking Z to FWD

Click OK in the xTm: Link Z to FWD dialogue if reasonable focus is achieved.

After a successful linking Z to FWD

Now the WD (displayed on the image data bar) is linked with the Z coordinate shown on the UI under Stage > Coordinates. This will allow the software to know the distance from the top of your sample to the bottom of the pole piece, and also prevent any accidental collision between the pole piece and your sample.

When the Link sample Z to Working Distance button appears like or , you need to redo the focus and Link sample Z to Working Distance.

means effective Link sample Z to Working Distance.

6. Move to the highest part of your sample. Zoom-in/magnify to about 2,000X and focus the image. Click on the Link sample Z to Working Distance button again.

This will allow the software to know the distance from the top of the highest part of your sample to the bottom of the pole piece, and also prevent any accidental collision between the pole piece and your sample.

You can raise the sample height, by typing a target height (e.g. 4 mm, or larger for non-flat surfaces) in the Z coordinate and click on the Goto button. Watch the CCD live view of the Chamber to make sure there is enough clearance above the sample.

Before clicking the Goto button to raise the stage, make sure that only Z coordinate is selected for moving, i.e., ticked in the square box.

The eucentric height for this system is 4 mm, which is required for FIB applications. However, for SEM imaging, 5 mm WD should be sufficient for most samples. Additional distance offers additional safety.

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The Stage can also be raised or lowered by click-holding the middle mouse button and moving it up or down in un-paused Chamber view quadrant.

Raise up Lower down

7. At higher magnifications, focus the image and click on the Link sample Z to Working Distance button again to obtain more accurate distance between the sample surface and the bottom of the pole piece.

Always focus and redo Link sample Z to Working Distance when the Stage has been moved by millimeter distance or further.

8. Stage moves: -75 mm to +75 mm for X and Y; 0 mm to 10 mm for Z.

When moving to a saved Stage position, Z axis might move as well. Therefore, to avoid lifting the sample into pole piece, make sure Link sample Z to Working Distance is done or Z axis is pinned before moving to a saved Stage position.

9. Stage rotation: 0° to 360°

Top view of a sample holder in the chamber as a rotation guide.

10. Stage tilt: -10° to 57° at 4 mm working distance

DO NOT re-link Z to WD when sample is tilted.

DO NOT tilt if WD<4mm is used.

Be careful when tilting large samples.

Only apply FIB applications to the highest surface of your sample. Otherwise the higher surface of your sample might touch the pole piece when tilting, or touch the Pt GIS needle when doing Pt deposition.

e-b

eam

sca

n di

rect

ion

Chamber door

Holder locking screw 0o

90o x

x 180o x

270o x

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G. Optimizing imaging conditions

1. Center a sharp feature of the sample in the e-beam quadrant.

2. Select a High Voltage and Beam Current that are suitable for the sample and imaging purpose.

Large High Voltage and small Beam Current are good for high resolution imaging with conducting hard materials.

For non-conducting or beam-sensitive samples, small High Voltage and Beam Current are desired.

For EDS data collection, the selected High Voltage should be 2.5 to 10 times of the interested peak energy. Beam Current should be chosen such that sufficient X-ray counts (1,000 cps to 40,000 cps) can be achieved but the Dead Time is below 50%.

3. Focus the live image in the e-beam quadrant. If the centered feature shifts during focusing, it means the Lens Alignment needs to be corrected.

Click on to bring up the Direct Adjustments window.

Under the Beam tab of the Direct Adjustments window, click on the Crossover button (yellow) to check if the source (live image of the beam) is reasonably centered. If not, center the source by dragging the cross center in the Source Tilt box to a newer location. If centered, click on the Crossover button (grey) again to exit source correction mode.

Under the Beam tab of the Direct Adjustments window, click on the HV Modulator button (yellow) to check if the Lens Alignment needs correction. If the feature in the live SEM image wobbles in and out of focus but does not move, no correction is needed. If it does move, minimize the move by dragging the cross center in the Lens Alignment box to a newer location. Once satisfied with the correction, click on the HV Modulator button (grey) again to exit lens correction mode.

4. Correct the image stigmation by turning the Stigmation X and Y knobs on SEM control panel to improve image quality. If the centered feature shifts during stigmation correction, Stigmators need to be centered.

Under the Stigmator Centering tab of the Direct Adjustments window, click on the Modulator X button (yellow) to check if Stigmator Center X needs correction. If the feature in the live SEM image moves, minimize the move by dragging the cross center in the Stigmator Center X box to a newer location. Once satisfied with the correction, click on the Modulator X button (grey) again to exit. Repeat for Modulator Y.

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5. Repeat steps 3 and 4 for better results.

6. It might be necessary to repeat steps 3 and 4 for each selected High Voltage and Beam Current.

7. When switching detectors and changing magnifications, it is also necessary to repeat steps 3 and 4.

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H. Obtaining images

1. Focus and stigmate on the area of interest at a desired magnification.

At low magnifications, ETD (regular secondary electron detector) is usually activated under the Field-Free mode (SRH) when un-pausing the e-beam quadrant for the first time after sample loading.

Move to an area of interest by using the joystick, double-clicking in the live SEM image, or double-clicking in the Nav-Cam photo (the navigation quadrant).

To avoid moving the Stage, Beam Shift can be used to image an adjacent location of the sample, achieved by turning the Beam Shift X and Y knobs on the SEM control panel, or dragging the cross center in the Beam Shift box.

Changing Scan Rate can help increase image quality, allow easier focus, or reduce image deformation.

Using the Reduced Area scan allows adjustment changes to be seen easier and faster.

2. Try moving to different areas on your sample before taking a final image, charging, sample shrinkage, and chemical effects in small areas can distort images.

3. When you obtain an acceptable image, press F2 to start a slow scan for a high quality image.

At the end of the slow scan, a Save Image window will appear. Or go to File>Save as to load the Save Image window.

Save images in the designated folder on the Support PC (My Network Places>\\Spc-hvm79\).

4. For high resolution imaging (UHR mode), you can use the through lens detector (TLD) under the immersion mode. Before switching to the immersion mode, the sample needs to be within the specified settings:

NEVER image magnetic samples under immersion mode.

Working distance smaller than 8 mm

Magnification above 1,600X

5. Switch to the immersion mode by clicking on the SEM mode drop down arrow and selecting Mode 2: Immersion.

The SEM mode drop down menu

6. Focus and stigmate the image.

Link Z to FWD again

You may need to do some corrections in the Direct Adjustments window.

7. When you obtain an acceptable image, press F2 to start a slow scan for a high quality image.

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At the end of the slow scan, a Save Image window will appear. Or go to File>Save as to load the Save Image window.

Save images in the designated folder on the Support PC (My Network Places>\\Spc-hvm79\).

8. When done with the Immersion mode, switch to the Field-Free mode.

If the image quality becomes very poor, check under detectors to see if ETD is ticked, as switching from the immersion mode to the Field-free mode doesn’t always lead to switching from TLD to ETD and TLD under the Field-free mode sometimes gives very bad imaging contrast.

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I. Ending the session

1. Make sure EDAX detector cooling is off.

If the EDAX cooling indicator is in red, the cooling is off.

On the EDAX PC, if TEAM is running, the sign indicates the cooling is off. Ok to Vent under Detector Status should be in green.

2. Make sure the GIS needles are retracted and the GIS heaters are off.

The GIS control is under the Patterning tab . Right-click on a GIS system to bring up a menu for switching the heater on/off. A ticked box indicates the needle is inserted.

3. Make sure the Easylift probe is retracted. The EasyLift control panel is under the Navigation tab .

Needles retracted, heaters off

EasyLift probe is inserted

EasyLift probe is retracted

Pt dep heater on but needle retracted Pt dep heater on and needle inserted

EDAX cooling indicator

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4. Make sure stage tilt is zero (check under the Navigation tab ), and the clearance between the pole piece and stage should be 4 mm or more (in the Chamber view quadrant).

5. Make sure the stage bias is switched off, i.e. the On button is not yellow.

Beam Deceleration control is under the Beam Control tab .

6. Make sure the High Voltage is off for both electron and ion beams, i.e. the Beam On button is not

yellow, and the stage is unlocked (lower right corner of the UI).


Click on the ion beam quadrant and check under the Beam Control tab .

A quick checklist before venting:








7. Click on the Vent button to vent the chamber. Click Yes on the xTm: Vacuum message dialog.

Stage unlocked

Ion beam HV off

Ion source ready

Ion beam HV off


e-beam HV off

Stage Bias unavailable Stage Bias off

Zero tilt

Sample surface is below the 4 mm bar

Clearance 4 mm

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Vent and then Yes

8. After 2-3 minutes of venting, the chamber will hiss loudly. When the hissing sound stops and the chamber icon (lower right corner of the UI) turns grey, the chamber door is ready to open.

chamber is vented.

9. Click on the Chamber view quadrant, and go to Window > Large Image Window to bring up the full screen CCD live view in Control PC monitor 2.

10. Open the Chamber door gently while watching the CCD live view of the Chamber.

11. Put on gloves! Gently loosen the locking screw and carefully remove the sample holder/stage from the holder/stage support.

12. Close the chamber door gently while watching the CCD live view of the Chamber.

13. Press the Pump button to pump down the Chamber, and apply a gentle push on the chamber door for a few seconds. When the chamber is pumped out the SEM icon (displayed under Status) will turn green.

While waiting for vacuum, clean up the sample preparation area.

14. Log out of the xT microscope UI by going to File>logout.

Users with designated Windows account need to log back in Windows as general_user/helios and start the xT microscope server and UI.

15. Copy data from the Support PC to your storage devices and remove the data from the Support PC.

Perform a virus scan on your storage devices using OfficeScan before copying data. NEVER insert a flash drive into the Control PC.

16. Finish logging in the logbook.

Date; Name; Time In/Out; Detector Used (SEM, SEM/EDX, SEM/FIB, SEM/CBS, SEM/STEM, cryo-SEM, cryo-SEM/EDX, cryo-SEM/FIB); and if there were any problems while using the tool.

17. Turn off the room lights and leave.

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J. Focused Ion Beam (FIB) work- Eucentric Height

1. Make sure the sample is suitable for FIB work (e.g. reasonably flat surface, firmly fastened on SEM stub, reasonably conductive…). And make sure the Chamber vacuum is good to continue (< 4x10-5 Torr).

2. Start to warm up the Ion source by clicking on the Wake Up button under the Beam

Control tab . This will allow warming up of the Ion source (~10 min) and opening of the column valves for both Ion and Electron Beams if the source is ready.

The Ion Emission Current will be stabilized at 2.0±0.2µA and then the Beam On button will become yellow. While waiting for the Ion Source to be ready, the Electron Beam can be used for imaging.

3. Bring the area of interest to the Eucentric height.

Make sure to Link sample Z to Working Distance with zero sample tilt.

Move the sample to 4 mm Working Distance (i.e. linked sample Z)

Go to the area of interest and center at an easily identifiable micron-size feature at ≥ 3500 X magnification.

Tilt the sample to 7°.

If the identified feature moves away from the center cross, use the Sample Z adjuster to move sample up or down until the identified feature is back to the center cross.

Linked sample Z

Sample Z

adjuster

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Tilt the sample to 52°.

If the identified feature moves away from the center cross, use the Sample Z adjuster to move sample up or down until the identified feature is back to the center cross.

Return the sample tilt to 0°, if the identified feature is still centered, or within 1 µm distance from the center cross, the eucentric height adjustment is good. Z (i.e. WD) should be around 4.10±0.5 mm.

4. Tilt the sample to 52°.

5. Under the Beam Control tab , make sure electron beam shift is set to zero.

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6. Click on the button to allow e-beam and Ion-beam images alternatively refresh. 7. Click on the Ion-beam quadrant.

8. Under the Beam Control tab , check Couple Magnifications to allow e-beam and Ion-beam images to change magnification at the same time.

9. Under the Beam Control tab , select the lowest Beam Current (either 1.1 pA or 2 pA, whichever available) and the largest High Voltage 30.00 kV (currently only 30 kV beams are aligned)

10. Set to a short beam dwell time, e.g. 300 ns and un-pause the Ion Beam quadrant to bring up a live image.

If image is not clear enough, longer dwell times can be tried. However, this is sample-dependent.

11. Adjust stigmators X and Y, and focus the Ion Beam to optimize the live image.

12. If the identified feature in the Ion-beam quadrant is not centered, adjust the Ion beam shift to center the feature.

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K. Focused Ion Beam (FIB) work- Pt Deposition and Milling 1. Double-check if the area of interest on your sample is at the eucentric height before you can start the

FIB milling process.

This should be done when moving to a new area of interest on the sample more than 500

m away or moving to an adjacent sample!

2. If your sample surface is beam-sensitive and important to your work, then you need to do electron

beam induced Pt deposition. Otherwise, this can be skipped.

A blanket metal protection layer, e.g. 10 nm Ir or thicker, could help skip this step, but it

might not be suitable for all samples.

If you are planning on adding a thick protective layer, then you should consider a thin layer

of pt deposition using the electron beam so that ion beam snapshotting does not damage

your surface.

Once you have a thin layer, you can deposit more platinum using the ion beam before you

start FIB milling.

Doing the deposition in two steps will save you some time, since deposition using the ion

beam is significantly quicker than the electron beam.

2.1 Set sample tilt at 0, i.e., the electron beam normal to the sample surface.

2.2 Highlight the electron beam quad.

2.3 Select a high current and low kV beam, and achieve reasonable image quality.

Suggested current and voltage are 1.6 nA or higher and 2 kV, respectively. However, other

beam conditions work too.

A high current decreases depositing time. A Low voltage reduces heating on sample

surface.

2.4 Go to the Patterning tab .

2.5 Click on the drop-down list on the Select Pattern Type , select a desired shape, and click on

it. Then the icon becomes yellow and the selected shape is displayed in the icon.

For electron beam induced Pt deposition, the rectangle shape is selected.

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2.6 Go to the e-beam quadrant, left-click&hold and drag a rectangle box to over the area of interest, and

then release the mouse button.

This rectangle box can be readjusted in size and repositioned if necessary.

Be careful to avoid any double-click in the quadrant that will lead to a stage move!

This can be done while the quadrant is either paused or under live scan.

2.7 Under the Patterning tab , click on the Basic subtab. For Application, choose to Pt dep surface

in its Value dropdown list. Green highlight on the box means the platinum deposition is selected.

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2.8 Below the Application setup, X, Y and Z sizes can be typed in with desired numbers.

X size and Y size define the coverage area while Z size defines a nominal thickness of the Pt

protection layer.

X size is suggested to start with 10 µm, Y size with 1 to 2 m and Z size with 0.1-0.2 m.

Larger or smaller sizes are both welcome to try, depending on the complexity and size of

area of interest. Larger sizes require longer deposition time.

The Time Value on this page indicates how long the Pt deposition will take under selected

conditions. In general, if it is longer than 10 minutes, the beam current should be increased

or the pattern size should be reduced to shorten deposition time.

2.9 Click on the e-beam quadrant if it wasn’t highlighted and double check if it is safe to insert the Pt

deposition gas supply needle.

The Pt deposition gas supply needle must be inserted only after the area of interest

(sample) is confirmed at the eucentric height.

2.10 Under the Patterning tab , find the Gas Injection window. Insert the Pt deposition gas supply

needle by clicking on the green box next to Pt dep. A tick sign will be in display.

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The Pt dep source should show “Warm” status when the sample chamber vacuum is ready.

If it shows “Cold”, the Pt deposition gas supply is not ready. Right click on “Cold” will bring

up an option for warming up the supply. The warming up procedure takes about 1-2

minutes.

2.11 Un-pause the e-beam quadrant to inspect any substantial movement of the area of interest.

For a large movement, such as loss of the area of interest in the view, it could mean a

needle touch on the sample. User(s) must stop work and find a tool owner for tool

inspection.

In most cases, there will be unnoticeable or very small movement. If necessary, the Pt

deposition pattern can be repositioned to match the area of interest.

2.12 Select the pattern and click on the Play button to start the Pt deposition.

Sometimes a window pops up asking to recalculate the deposition time. This is due to a current

fluctuation. Click on Recalculation, and press play again to start the Pt deposition.

If the Pt deposition gas supply needle is not currently inserted, a window pops up asking to

insert it. Click on Yes if safe to do so.

2.13 Once the Pt deposition is complete, retract the needle by clicking the green box next to Pt dep. The

tick sign should be gone.

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2.14 Select the desired imaging condition (e.g. 10 kV and 50 pA). Un-pause the e-beam quadrant and

inspect the deposited Pt pattern.

The pattern quality is not a key concern at this point. However, a well-defined Pt pattern

indicates a stable sample that usually presents less challenge in later steps.

3. Set magnification at 3500-5000 times. On the Beam Control tab, find and check the box next to

Couple Magnifications.

4. Set the sample tilt at 52, i.e., the ion-beam normal to the sample surface. Observe the move of a

centered feature, and improve eucentric height if necessary.

Any distinguishable feature can be used for this purpose, but the Pt deposition pattern by

e-beam is a good one.

Make sure the image in the electron beam quadrant is still focused.

5. Click on Ion-beam Quadrant. On the Beam Control tab, if the ion beam is not on, click on the Beam On

button.

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If the FIB source wasn’t on, i.e., the bar indicator above the Beam on button is not green,

the system will warm up the FIB source first. This might take 5-10 minutes.

If the FIB source was found off, this step can be performed a bit earlier.

6. Select 30 kV and 1.1 pA (or the lowest available current) for the ion beam.

7. Snapshot an image in the ion beam quadrant by clicking this button , or pressing the F4 key.

The snapshot should be done with the lowest current and as less repeat as possible, to

minimize sample damage.

Other currents and voltage values can be tried too. The ion beam is aligned at 30, 16, 5,

and 2 kV with all available currents.

8. Use beam shift in the Ion beam quadrant to allow the same feature centered in the e-beam quadrant

to be also centered in the ion-beam quadrant.

To do this, hold the Shift key first, in the meantime left click on and drag the same feature

that is already centered in the e-beam quadrant, to the center cross in the ion beam

quadrant.

This only moves the ion beam to center the desired feature in the ion beam image, but not

the stage itself.

Take a snapshot in the ion beam quadrant to confirm that the desired feature is centered.

Repeat this procedure at a slightly higher magnification for more accurate centering.

Note: sample not well mounted could experience difficulty at this step.

9. Focus the image in the ion beam quadrant quickly at the lowest current and a short dwell time.

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Beam optimization with the stigmator X and Y adjustments are often needed. To avoid

unwanted milling in the area of interest, enable the reduced area function, re-size

and move it to a feature near the area of interest.

If there are no features, the edges of a purposely made milling trench can be used for

focusing and stigmator adjustments.

Make sure the focus is achieved on the same surface level as your area of interest.

This should be done quickly since the material gets milled rapidly, and the features to focus

on can be lost right away.

The image scanning speed, associated with the beam dwell time, should be fast to

minimize milling during beam optimization, but also reasonable for observing focus

change.

Confirm that the image in the electron beam quadrant is still in focus, and centered with

the same feature as that centered in the ion beam quadrant.

Always remember to reduce the current to minimum when taking a preview image.

10. Center the area of interest and deposit a platinum protection layer on a selected area using the ion

beam.

10.1 Set sample tilt at 52, i.e., the ion beam normal to the sample surface.

10.2 Highlight the ion beam quadrant.

10.3 Select an ion beam current between 8 pA and 80 pA, and snapshot an ion beam image.

Higher current will deposit platinum faster. However, a current higher than 0.43 nA will

end up milling the surface instead of deposition.

The suggested current is 40 pA or 80 pA but if the deposition timer is longer than 10

minutes, 0.43 nA can be used..

Larger protection areas require longer deposition times. Therefore, it might not be possible

to set all deposition tasks under 10 minutes, regardless of the current used.

10.4 Go to the Patterning tab .

10.5 Click on the drop-down list on the Select Pattern Type , select a desired shape, and click on

it. Then the icon becomes yellow and the selected shape is displayed in the icon.

In general, the rectangle shape is selected for the protection layer. However, other shapes

can be used too.

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10.6 Go to the ion beam quadrant, left-click&hold and drag a rectangle box to over the area of interest,

and then release the mouse button.



This can be done while the quadrant is either paused or under live scan, but live scan

causes unwanted milling.

If a protection layer by electron beam was achieved beforehand, then this box should

roughly match that.

10.7 Under the Patterning tab , click on the Basic subtab. For Application, choose to Pt dep in its

Value dropdown list. Green highlight on the box means the platinum deposition is selected.

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X size and Y size define the coverage area while Z size defines a nominal thickness of the Pt

protection layer.

X size is suggested to start with 10 µm, Y size with 1 to 2 m and Z size with 0.5-1.0 m.

However, these all can be adjusted to achieve the best results.

Larger or smaller sizes are both welcome to try, depending on the complexity and size of area

of interest. Larger sizes require longer deposition time.


conditions. In general, if it is longer than 10 minutes, the beam current should be increased or

the pattern size should be reduced to shorten deposition time.

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10.9 Click on the ion beam quadrant if it wasn’t highlighted and double check if it is safe to insert the Pt

deposition gas supply needle.

The Pt deposition gas supply needle must be inserted only after the area of interest

(sample) is confirmed at the eucentric height.

10.10 Under the Patterning tab , find the Gas Injection window. Insert the Pt deposition gas supply

needle by clicking on the green box next to Pt dep. A tick sign will be in display.

The Pt dep source should show “Warm” status when the sample chamber vacuum is ready.

If it shows “Cold”, the Pt deposition gas supply is not ready. Right click on “Cold” will bring

up an option for warming up the supply. The warming up procedure takes about 1-2

minutes.

10.11 Snapshot an ion beam image to inspect any substantial movement of the area of interest.

For a large movement, such as loss of the area of interest in the view, it could mean a

needle touch on the sample. User(s) must stop work and find a tool owner for tool

inspection.

In most cases, there will be unnoticeable or very small movement. If necessary, the Pt

deposition pattern can be repositioned to match the area of interest.

10.12 Select the pattern and click on the Play button to start the Pt deposition.

Sometimes a window pops up asking to recalculate the deposition time. This is due to a

current fluctuation. Click on Recalculate, and press play again to start the Pt deposition.

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If the Pt deposition gas supply needle is not currently inserted, a window pops up asking to

insert it. Click on Yes if safe to do so.

10. 13 Once the Pt deposition is complete, retract the needle by clicking the green box next to Pt dep.

The tick sign should be gone.

10.14 Snapshot an ion beam image to inspect the deposited Pt pattern.

The pattern quality is not a key concern. However, a well-defined Pt pattern indicates a

stable sample that usually presents less challenge in later steps. And the ion beam

deposited Pt pattern appears sharper than an electron beam deposited pattern.

The platinum deposition by ion beam can be observed through electron beam imaging,

using the iSPI function under Patterning End Point Monitor if taught to do so.

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11. To mill a cross section with FIB, make sure the ion beam quadrant is highlighted. Go to the Patterning

tab to define the trench to be milled.

Double check if the sample is still at the eucentric height. Samples not properly mounted

might drift far over a long period of pattern-processing time.

Double check if the same feature is well centered in both the electron beam and ion beam

quadrants.

Retaking a snapshot in the working quadrant should be done every time when the

magnification is changed.

11.1 Click on the drop-down list on the Select Pattern Type , select a desired shape, here the

Regular Cross Section to cut a cross section, and click on it. Then the icon becomes yellow and the

selected shape is displayed in the icon.

11.2 In the ion beam quadrant, left-click&hold and drag a rectangle box, which defines a stairway mode

milling that leads to a trench gradually deeper at the cross section, to over the area of interest, and

then release the mouse button.



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This can be done while the quadrant is either paused or under live scan, but live scan

causes unwanted milling.

If a Pt protection layer was achieved beforehand, then this box should roughly align with

the front of that protection layer.

11.3 For trench milling, the ion beam current needs to be reasonably high.

A value for current in the nA range at 30 kV should be good in general. This can vary

depending on the samples. Beam sensitive samples requires smaller currents, but resulting

in longer trenching times.

Always take a new snapshot after changing the beam conditions. The high-current ion

beam usually doesn’t need to be re-focused unless it is really bad.


X size and Y size define the trench milling area while Z size defines a nominal depth of the

trench.

X size is suggested to start with 10 µm, Y size is related to how deep to observe the cross

section by the electron beam, 1 m and above is a good start but a larger value is needed

to see deeper. Z size is related to the sample, i.e., how deep one would expect to see

structures. Any value between 1 and 10 m is common. These all can be adjusted to

achieve the best results, according to user’s needs.

Larger or smaller sizes are both welcome to try, depending on the complexity and size of

area of interest. Larger sizes require longer deposition time.


conditions. In general, if it is longer than 10 minutes, the beam current should be increased

or the pattern size should be reduced to shorten deposition time.

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11.5 The trench milling procedure can be monitored using the iSPI function under Patterning

End Point Monitor if taught to do so,

The iSPI function will direct the electron beam quadrant to take an image at the pre-set time

intervals (max. at 30 s). Every time when the electron beam does a scan, the milling stops, so

this iSPI function can affect the milling time, i.e., leading to a longer wait time.

Set up the iSPI function, make sure iSPI > On is checked and select a desired time interval (max.

at 30 s).

Select the electron beam quadrant, and un-pause the electron beam. Note: The iSPI images are

NOT saved automatically. They are images for users to observe the milling progress, and make

decisions if needed.

11.6 Select the milling pattern in the ion beam quadrant. Press Play to start milling.

The material removal is done in a stairway manner starting from the bottom side of the

rectangle pattern. This can be changed under Pattern > Basic > ScanDirection, but should be

always “Bottom To Top” for simple cross section

tasks,

11.7 After trenching, the cross section usually needs a polish for better image quality. Under Pattern >

Shape Selector, choose Cleaning Cross Section, and place a milling box next to the cross section

edge. Set up milling dimensions, select a polish current (equal to or smaller than the trenching

current), and press Play .

Take a new snapshot and double check if the same feature is well centered in both electron

and ion beam quadrants.

The Y direction of the polish pattern should be enough to start before the cross section edge,

as well as mill into the protected layer.

Polishing depth (Z) should be deeper than the trench to obtain a steep and high quality cross

section. If “curtaining effects” is observed on the cross section, deeper polishing is needed.

Higher currents mill faster, but the non-uniform milling could occur with high milling currents.

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11.8 Set the ion beam current to the minimum so that the sample won’t get substantially milled in case

the ion beam is accidentally un-paused.

12. Start imaging the polished cross section with the electron beam. Re-polishing might be needed if the

cross section is not smooth enough, or if it gets contaminated by beam induced deposition.

13. The FIB source can be left on until the end of the tool session. By the end of the session, click on

Sleep if there is no immediate FIB user after you, or confirm with a staff member.

The following screen capture shows that the FIB source is switched off.

14. Tilt the stage back to 0 degrees and finish the session as you would with SEM.

13. Once you finish FIB work,

Pause the Ion Beam quadrant.

Set to the lowest Ion Beam Current.

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Turn off the Ion Beam (a grey Beam On button, but source can be still available).

Retract the Pt GIS needle if it was used.

Return the sample to 0° tilt.

If you are the last one of the week using the Ion Beam, turn off the Ion Source by clicking on

the Sleep button under the Beam Control tab .

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L. Setting up cryo-SEM conditions: Helios SEM Stage and Chamber

1. Book sufficient tool time and let other users know that regular SEM/EDX/FIB operations will be unavailable during cryo-SEM.

Currently, all bookings for cryo-SEM are done through the tool owner. And the tool owner will send an email notification.

2. Make sure there is sufficient liquid nitrogen supply.

Remind tool owner to prepare sufficient liquid nitrogen. 3. Perform the following checklist.








4. Vent the SEM Chamber if safe to do so.

5. Put on gloves!!!

6. Open the Chamber door gently and move all coordinates (X, Y, Z, T, R) to zero, or Home the stage.

7. Remove the cross-shaped SEM stage support and its locking collars.

8. Mount the cryo-stage base and the cryo-stage dock.

The pen marks on the SEM stage, cryo-stage base and cryo-stage dock should line up.

All the locking screws should be reasonably tightened but not over-tightened.

Connect the cryo-stage grounding wires to the SEM stage. Tighten the grounding screw to ensure sufficient conductivity.

Make sure the cables and Teflon tubes connecting to the cryo-stage dock are not entangled with cables of any other SEM detectors.

Make sure the Teflon tubes connecting the cryo-stage are not kinked. 9. Move the Stage to the Cryo loading position, a saved stage position for loading cryo samples onto

the cryo-stage dock.

10. Lock the Stage rotation.

11. Never Take Nav-cam Photo when a cryo stage is in place.

12. Move the anti-contamination cold plate to the close proximity to the pole piece.

Loosen the cold plate locking screw to make the plate easier to move. And tighten the locking screw once the plate is in targeted place.

Be careful not to touch the pole piece with your finger or the cold plate.

Make sure the Teflon tubes connecting to the cold plate are not kinked. 13. Close the Chamber door slowly and watch the Chamber live view to make sure there is sufficient

clearance below the pole piece.

14. Pump down the SEM Chamber.

15. Wait for the Chamber vacuum to be ready, i.e. < 4E-5 Torr.

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M. Setting up cryo-SEM conditions: cooling by Quorum control

1. Checklist.

Cryo stage dock is installed on Helios and well grounded.

Anti-contamination cold plate is in place next to the Helios pole piece.

Helios Chamber vacuum is ready, i.e. < 4E-5 Torr.

In-house nitrogen supply is available.

The transfer rod on the transfer device is reasonably greased/oiled.

Sufficient liquid nitrogen supply. 2. Start the aQuilo program and pump down the Quorum sample preparation chamber.

This is usually done the night before cryo SEM session to minimize waiting time. 3. Once the Quorum sample preparation chamber vacuum is ready, i.e. < 4E-5 Torr, click on the Startup

button of the aQuilo program to bring up a setup window.

If the aQuilo program was running and the Startup button is not active, click on the Shutdown button and wait for the Startup button to be active.

4. On the setup window, check log vacuum and click on the Automode button to proceed. A Startup reminder: please configure the microscope for cryo operation will show up.

5. If the cryo-stage dock and anti-contamination cold plate are set in place and SEM Chamber is pumped down, click Ok. A reminder: Please fit the pump out valve to CHE300 will show up.

6. Fit the pump out valve and rotate the pickup screw clockwise until it stops. Then click Ok. A reminder: Please Open pump out valve will appear.

7. Pull up the pickup screw on the pump out valve and clip the yellow clamp on the pickup screw. Then click Ok. The system starts to pump the isolated lines and purge the high purity nitrogen lines.

8. This process takes 20 minutes. Fill the liquid nitrogen dewar while waiting.

9. After 20 minutes, a reminder; Please close the pump out valve will appear.

10. Remove the yellow clamp, push the pickup screw down and rotate it clockwise until feeling a stop. Counter-clockwise rotate the screw to release the valve. Click Ok to vent.

11. Pull up the pickup screw to hear a vent sound. Then click on Ok.

12. Remove the pump out valve from CHE300.

13. Check if the set temperatures are correct.

14. Put CHE300 in the liquid nitrogen dewar, and then click OK.

15. Click on Auto buttons and wait for the temperatures to reach set temperatures.

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N. Preparing cryo samples

1. The sample transfer device has one inch diameter, samples wider than 20 mm will not fit.

2. If the sample is too big, it might explode when loading into vacuum.

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O. Loading cyro samples

1. Four key conditions before transferring cryo samples from the cyro sample preparation chamber into the SEM chamber.

Both electron and ion beams are off.

Move the Stage to the Cryo loading position.

The temperature difference between the SEM Stage and the sample preparation stage is within 1-2 C°.

The pressures in the SEM Chamber and the Quorum sample preparation chamber are similar.

2. NEVER rotate the Stage when the SEM is in the cryo mode.

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P. Unloading cryo samples

1. Turn off the Electron and Ion beams.

2. Return sample to the cryo loading position.

3. Make sure the temperature difference between the SEM Stage and the sample preparation stage is within 1-2 C°.

4. Make sure the pressures in the SEM Chamber and the Quorum sample preparation chamber are similar.

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Q. Elemental analysis using the EDAX detector

1. Manually drive/insert the EDAX detector to the optimal analysis position.

When not in use, the EDAX detector should be retracted to the 200 mm position (read from the back of the detector), to avoid possible damage/contamination by plasma cleaning, FIB and cryo work.

A white ring marker should stop the detector at the 121 mm position, to avoid the detector being inserted too close to the pole piece.

If the user is not comfortable moving the EDAX detector, please ask the tool owner for help.

The EDX detector kept out. The EDX detector reeled in.

2. Link Z to working distance if not done so.

3. For optimal signal collection for EDX a working distance of 5 mm is needed.

4 mm is good as well if high resolution or FIB work is done.

4. Select appropriate beam energy and current. The detector deadtime should be around 30%.

Beam energy: 2.5 to 10 times of the peak positions of concerned elements.

Beam current: lower for beam sensitive samples but lead to long acquisition time and noisy spectra.

The deadtime will change with selected beam current and significant variations in the sample high.

5. Reel the detector in to the correct position of 120 mm (read from the back of the detector).

Note that the detector still works when it is out. If your work requires a surface level

analysis, and your sample can handle higher current, it is safer to keep the EDX detector

out to avoid contamination on the detector.

6. All detectors can be used for EDX since the EDX detector has its own magnetic repulsion.

The white ring marker

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7. Open team software on the EDX computer. The username and password are general_user and helios,

click on log in.

If the software is already open, you just need to log in.

8. Click on create project or start with an already existing project.

9. Hover the cursor over the triangle on the top right where it says Advanced Properties and click on it to

make it solid.

10. Go to the EDS detectors window and make sure Det 1 box has a checkmark. Under Octane Super click

on Det 1 - Detector Status and click on cooling off in red, it will change to cooling on. Wait until cooling

on is turned green, meaning cooling is complete and a temperature of -30 Celsius is reached.

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11. Check the bottom bar and make sure the information displayed there about magnification, kV and

working distance is correct. If not, restart the program.

Sometimes there will be a mismatch between the magnification, if it is less than 1% ignore.

If the mismatch is more than 1% check the scanning dwell time and try making it faster.

Also try increasing the number of pixels in the image.

For images with high number of pixels, for example 3072x2048, the magnification between

the SEM image and the EDS will be off by more than a few percent. In this case, just check

to make sure that a size of a specific feature on the SEM and EDS images are the same size.

If this doesn’t work log off and log back in the EDX computer.

12. Hover over Project Content window on the left. Click on the triangle to make it solid.

13. At the top, under Point Analysis tab, click on the triangle on the Image Area to see the image setting.

You can change the setting and image resolution.

Don’t check the drift correction box.

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14. Click on image area tab itself to obtain an image.

15. Click on the point of interest on the image, or click and drag for an area of interest.

To delete one of these, select the box or point, hover over the box and left click.

You can choose multiple points or areas, and get a spectrum for each individually.

16. To collect a spectrum, open the Collect Spectrum options by clicking on the triangle. There is no need

to change anything but the seconds. Then click on Collect Spectrum tab itself to start recording. The

spectrum for each point or area can be individually chosen by double clicking on them in the Project

Content window.

To change the energy range of the spectrum:

o On the bar to the left of the spectrum, hover over the first icon and click on Customize

to change the range of the spectrum.

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o Holding the control key and holding right click on the spectrum and dragging changes

the size of the spectrum.

17. Click on the Elements tab on the left to open up the periodic table. Hover over the elements to see

their reference spectrum. Select or deselect the elements, press Ok.

To see elemental suggestions, left click on a peak and hover the mouse over the question mark.

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18. Click on the Manual Background Adjustment on the left bar to remove the background noise. Hover

over the x-axis under the area you want removed and left click. To bring the removed area back,

highlight it and press delete on your keyboard.

To zoom in on a region of a spectrum, left click and drag. To go back press the icon of

customize.

You can adjust the size of the removed area by holding left click on the edge of the removed

area and moving the cursor.

You can move the removed area by holding left click on it and moving your cursor.

19. Click on the Deconvolution button to deconvolute and check to see if a proper background subtraction

was done by making sure the fitted blue line matches the measured spectrum (shows up in red).

Otherwise redo the background subtraction.

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20. Once you are done editing, click on the Manual Background Adjustment again to get out of the

adjustment mode.

21. To see the quantification, click on the quantification window.

22. After you make all your changes, click on the Save icon (last icon on the left) to save changes to the

spectrum.

23. To move on to the spectrum of a different point, double click on the other point in the Project Content

window to the left and repeat the steps above.

24. Click on the Review Data tab and then click on Report to generate a report file.

If only one spectrum is selected, there will only be one report. To report on all the areas,

double click on the “area” parent folder and then click on report.

25. To save the report, go to Save drop down, and save as Microsoft Word 2007 file in the support

computer (save to your folder in the Z: SharedData).

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26. To start a new spectrum or mapping, click on Sample in the project content window. Then select New

Sample and click on Ok. You can write a name for the sample.

27. For mapping, click on the Mapping tab at the top, and then click on the Image Area to capture an

image.

You can adjust the resolution by pressing the triangle to open the drop-down option.

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28. Click on the triangle on Collect Map tab to adjust setting. You can adjust the map size by clicking and

dragging the lower right corner of the rectangle on your image.

Set the resolution, frame and dwell time.

Consider the number of pixels with selected resolution, and the collected data region size.

Mapping can take a very long time if you are not careful with these parameters. Dwell time is

the amount of time spent for each pixel, and the frame is how many times the mapping will

start a new frame to put on top of the old one.

The formula for getting the mapping time is [(# of pixels) x (dwell time) x (frames)].

If sample is not stable, increase frame and reduce dwell time.

29. When ready to start mapping, click on Collect Map and checkmark “confirm elements after preview” to

double check the elements of interest and change them if necessary.

Check the deadtime is around 30%. See step 4 for more information.

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30. Once the map is finished, Select the desired elements, and click Ok.

31. Once the mapping is complete, click on the Finish tab.

32. Proceed to the Review Data tab to look at the data. Under the Area below sample name double click

on Live Map, and click Report for each Live Map.

You can generate a report for one map at a time only.

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33. To finish:

Click on cooling on to change to cooling off.

->

Retract the EDX detector back to the original position.

Un-pause the chamber view and go back to normal SEM imaging.

Operating Procedure1,2,3 for the Helios NanoLab 650 SEM ...1 FEI Helios NanoLab 600 SEM/FIB Basic...

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Transcript of Operating Procedure1,2,3 for the Helios NanoLab 650 SEM ...1 FEI Helios NanoLab 600 SEM/FIB Basic...