Talos F200XUser guide

For reference only, not a substitute for training from CHANL staff.

1. Sample holder

2. Initial diagnostics

3. Loading Sample Holder

4. Talos-Flucam Interface

5. Setup and TEM Alignment: Z-align

6. Setup and TEM Alignment: Condenser lens and Condenser Stigmation

7. Setup and TEM Alignment: Direct Alignment (drop up menu)

8. Setup and TEM Alignment: Objective lens and Objective Stigmation

9. Velox Acquisition and Processing

10. Imaging: Ceta Camera on Velox Interface

11. Setup and STEM Alignment

12. Diffraction

13. Unloading Sample Holder

Table of Contents

Sample Holder: single tilt

• Wear gloves to prevent contamination.

• Be gentle and do not touch the brass holder assembly.

• Make sure the grid is dry.

• Use the sample loading tool (pin) to lift the clamp.

• Load grid in the slot on the holder. Sample side faces down when loading grid on the sample holder.

• Use to pin to rest the clamp on the grid.

• Gently tap the holder to make sure the grid is in place.

• Training on other sample holder (double tilt/Tomography) will be done as needed.

• Be gentle and avoid any form of contamination.

Initial diagnostics

• Green means go.

• Make sure the accelerator, column and detection unit status is green on the LED touchscreen.

• If anything is red, please contact CHANL Staff.

• If Nitrogen level is below 20%, please contact CHANL staff.

• Reset xyz and α /β tilts to zero before loading the sample.

Loading Sample Holder

• Watch link for sample loading: https://www.youtube.com/watch?v=HErGMLPlt7s

• Press Load Sample and follow instructions from the LED screen.

• Line the pin of the holder with the mark on the holder assembly and push all the way till the sharpie mark on the holder rod.

• Vacuum process will be initiated (red light on) and you should hear a the pump and a valve open.

• The display will prompt you regarding selection of holder (single tilt/double tilt/). Press Single tilt and wait for 300sec.

• Once ready (red light off), rotate the holder counter clockwise till it stop and gently push it in till it stops.

• Reset stage co-ordinates back to zero before operation.

• In the event of vacuum loss, please contact CHANL staff.

Talos-Flucam Interface:

Setup and TEM Alignment: Z-align

• Make sure the column vacuum is below 15 log.

• On the Talos Interface, press “ Col. Valves Closed”, so it turn grey.

• Under FEG Registers Select “200kV TEM” and click “Set”. It should recall all conditions set for 200kV TEM operation.

• Live image should appear on the Flucam viewer. Decrease magnification below 1000X to see the grid overview.

• Use the joystick on the right hand panel, to navigate x/y coordinates. Select a feature and increase magnification to a decent magnification around 54kX (in SA mode).

• Spread the beam evenly to cover the Flucam Viewer. Use the tracking ball on the left panel to control the beam shift in x and y direction.

• Press “Eucentric Focus”, this will bring the DV (defocus value) to a certain number (close to 585nm)

• Press “Wobbler”, the beam will wobble around the sample, press z axis ± to minimize sample movement or to bring the sample to a point of minimum contrast or eucentric height position.

• It is critical for the sample to be at eucentric height.

Setup and TEM Alignment: Condenser lens and Condenser Stigmation• For FEG register 200kV TEM, the Condenser 1 will be at

2000um. Condenser 2 will be at 150, it can be at 100, 70 and 40um (drop up menu on the right had bottom corner of the Talos Interface). Condenser 2 controls the brightness of the image.

• At a certain magnification in the SA mode, center the beam with the tracking ball and go through crossover (smallest spot of the beam) using the intensity knob on the left hand panel.

• Always be on the underfocus side of the crossover, i.e . spread the beam in a clockwise manner to illuminate the Flucamviewer.

• Condenser lens alignment: Using intensity knob, make sure the beam moves in and out as you go through crossover. If the beam sways in any directions, click adjust besides the Condenser 2 position and use the multifunction knobs (MF-x and MF-Y) to adjust the condenser lens to move beam in and out.

• Condenser Stigmation: At a certain magnification in the SA mode, condense the beam and make sure the beam in circular, if it is not, click Stigmator from the drop up menu then select condenser and use MF-X and MF-Y to make the beam rounded. Click none after adjustment.

• Exit out of the individual and the drop up menu to disable the multifunction knobs.

Setup and TEM Alignment: Direct Alignment (drop up menu)• Gun Tilt (generally not needed) for the FEG

register 200kV TEM

• Gun Shift (generally not needed) for the FEG register 200kV TEM

• Beam tilt pp X and Y, or pivot point X and Y: Condense the beam to crossover (a small spot) using the intensity knob. The beam will wobble, minimize the wobble and merge the spot to a single spot using the multifunction Mf-X and MF-Y for pp X and pp Y alignment.

• Beam Shift: At magnification close to 100kX, use multifunction MF-X and MF-Y to center the beam.

• Rotation center: At a decent magnification of around 100kX , monitor a feature, click “Rotation center” and minimize image shifts or the image should pulse in and out, using the multifunction MF-X and MF-Y knob.

Setup and TEM Alignment: Objective lens and Objective Stigmation• Introduce objective aperture to get optimum contrast (sample

dependent). Objective 60um and 70um does works well. Select them from the drop down menu in the aperture window.

• Objective lens alignment: Make sure the beam in not blocked by the objective as the beam goes through cross-over and illuminates the Flucam screen evenly. If it does block, click “Adjust” besides the objective aperture and use the multifunction MF-X and MF-Y to adjust the aperture.

• Objective Stigmation: Find amorphous region, grid or polymer layer, at a decent magnification above 100kX focus and observe the Fast Fourier Transfer FFT by clicking on the FFT option on the Flucam viewer. The FFT should be circular and should concentrically move in and out when you go in and out of focus. If the FFT appears oblique, click Stigmator from the drop up menu, then select Objective and use the multifunction MF-X and MF-Y to make sure the FFT is circular.

• Good idea to have the MF-X and MY-Y set to objective stigmatorand get in the habit of tweaking the objective stigmation to make the feature edges look crisp.

Velox Acquisition and Processing:

Imaging: Ceta Camera on Velox Interface • With the appropriate condenser aperture and objective aperture inserted, find area of interest , spread the beam clockwise to

illuminate the whole Flucam viewer.

• Focus using the focus knob, bottom part of the focus knob is for focus steps. You can change it for course and fine focus. Focus step 3 is good for relatively low magnification images. Change focus step for imaging at magnifications above 250kX.

• Focusing and alignment and change in magnification must be done on Flucam viewer.

• Click insert screen to start imaging with the Ceta Camera on the Velox acquisition interface.

• Velox acquisition and Velox processing windows should be open.

• Define folder in Velox Acquisition before imaging. Edit>Preferences>Autosave path. Find your folder and create new folder.

• Click Velox viewing to start imaging and Velox acquisition to acquire images.

Imaging

Imaging: Ceta Camera on Velox Interface • Parameters for pixel size and acquisition time can be changed for both viewing and acquiring images.

• Captured images will appear on the Velox acquisition window and you can also export images to your folder.

• EDS data can be obtained in the TEM mode by clicking the live EDS spectra and then by clicking the acquire EDS spectra icons. EDS spectra and its details will be saved in the Velox acquisition window. Make sure to keep conditions like magnification and aperture for condenser constant for reasonable quantitative estimation.

EDS

STEM Setup and Alignment:• Under FEG Registers Select “STEM spot 7” or “STEM spot 8”

and click “Set”. i.e condenser 2 aperture 70um and 80um. It should recall all conditions set for STEM operation.

• Diffraction spot should appear on the Flucam viewer. Center the spot by clicking Direct alignment and then Diffraction Alignment and by using the multifunction knobs MF-X and MF-Y.

• Velox interface should change to STEM mode. Click STEM viewer to start live imaging.

• Decrease magnification and use the Z-height on the right hand panel to bring the specimen to Eucentric height. Also, adjust Eucentric height for very high magnifications > 1 million X.

• This setup should be good for the FEG register for STEM.

• If needed check for the Ronchigram characteristics.

• To observe Ronchigram, pause live scan on the Velox. Change condenser aperture from 70um/80um to 150um. Center the Ronchigram in the Diffraction alignment mode using the multifunction MF-X and MF-Y knobs.

• Correct for condenser stigmation to get a circular Ronchigramby clicking condenser in the Stigmator mode using the multifunction MF-X and MF-Y knobs.

• Insert the desired condenser aperture and image using Velox.

Imaging: Ceta Camera on Velox Interface • Click HAADF to start imaging and Velox acquisition to acquire images.

• Can also obtain images in Dark Field2 (DF2), Dark Field4 (DF4) and Bright Field (BF) modes.

• EDS spectra from the field of view can be acquired by clicking EDS and EDS acquisition. Spectra and details will be saved in the Velox processing window.

• For EDS maps click on EDS mapping. For the set FEG register you can change spot size and condenser apertures to obtain optimum counts and obtain a decent visual contrast for the elements in context. Also a good idea is to select a certain area for drift compensation before running a map. For the set FEG register with drift correction and 5-10minutes acquisition should result in decent EDS maps.

ImagingEDS spectra

EDS MapsDrift correctionSpectral Region

Diffraction Setup and Alignment:• If you are planning to do diffraction, you should do so after

imaging so the alignment for FEG register 200kV TEM is already set.

• At a certain magnification focus the beam and press ‘Diffraction”

• Diffraction spot should appear on the Flucam viewer. Center the spot by clicking Direct alignment and then Diffraction Alignment and by using the multifunction knobs MF-X and MF-Y.

• Sharpen diffraction spot using the intensity knob.

• If spots are intense, Insert appropriate Selected area aperture

Unloading Sample Holder

• Watch link for sample unloading: https://www.youtube.com/watch?v=HErGMLPlt7s

• Close column valve.

• Go to the instrument and press Reset xyzαβ on the display screen.

• Press Remove Sample

• Pull sample holder straight from the holder assembly till it stops. Turn the holder clockwise till it stop and then gently pull it out.

• Reset stage co-ordinates back to zero.

• In the event of vacuum loss, please contact CHANL staff.