Cambridge ALD: Difference between revisions

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|company = Cambridge NanoTech (Veeco)
|company = Cambridge NanoTech (Veeco)
|description = Atomic layer deposition system
|description = Atomic layer deposition system
|location = Cleanrooms 1 & 2
|location = Cleanroom 1 (03.2.209A)<br />Cleanroom 2 (03.2.203B)
|primary = Martin
|primary = Harry
|secondary = Karolis
|secondary = Martin
}}
}}
Two nearly identical Savannah S100-like systems are used for atomic layer deposition of '''aluminum''', '''hafnium''', and '''titanium''' '''oxide'''.
Other material deposition alternatives at the [[Main Page|NBI cleanroom]]:
* [[AJA systems]] for sputtering/e-gun evaporation
* [[E-Gun evaporator]]
* [[Edwards evaporator|Edwards thermal evaporator]]
* [[Leica sputter coater]]
* [[MBE|Molecular beam epitaxy system]]


== Growth per cycle (GPC) monitoring ==
== Growth per cycle (GPC) monitoring ==


<gallery mode="traditional">
<gallery mode="packed" widths=500 heights=200>
Image:ALD1.png
Image:ALD1.png|ALD1 HfOx
Image:ALD2.png|
Image:ALD1AlOx.png|ALD1 AlOx
Image:ALD2.png|ALD2 HfOx
</gallery>
</gallery>


Line 23: Line 34:
! Deposited material !! Precursor !! ALD1 !! ALD2 !! Ref.
! Deposited material !! Precursor !! ALD1 !! ALD2 !! Ref.
|-
|-
| Hafnium oxide (HfOx, HfO<sub>2</sub>)|| <div class="toccolours mw-collapsible mw-collapsed width:400px" style="width:300px"> TDMAH <div class="mw-collapsible-content">tetrakis(dimethylamino)hafnium <br/> [(CH<sub>3</sub>)<sub>2</sub>N]<sub>4</sub>Hf <br/> [[File:TDMAH.png|246px]]</div></div> || style="background-color: #c6e0b4" | Yes || style="background-color: #c6e0b4" | Yes || [https://doi.org/10.1016/j.tsf.2005.05.050]
| Hafnium oxide (HfOx, HfO<sub>2</sub>)|| <div class="toccolours mw-collapsible mw-collapsed width:400px" style="width:300px"> TDMAH <div class="mw-collapsible-content">tetrakis(dimethylamino)hafnium <br/> [(CH<sub>3</sub>)<sub>2</sub>N]<sub>4</sub>Hf <br/> [[File:TDMAH.png|246px]]</div></div> || style="background-color: #c6e0b4" | Yes || style="background-color: #e0b4c6" | No || [https://doi.org/10.1016/j.tsf.2005.05.050]
|-
|-
| Aluminum oxide (AlOx, Al<sub>2</sub>O<sub>3</sub>) || <div class="toccolours mw-collapsible mw-collapsed" style="width:300px> TMA <div class="mw-collapsible-content">trimethylaluminum <br/> (CH<sub>3</sub>)<sub>3</sub>Al <br/> [[File:TMA.png|290px]]</div></div> || style="background-color: #c6e0b4" | Yes || style="background-color: #c6e0b4" | Yes || [https://doi.org/10.1134/1.1626763]
| Aluminum oxide (AlOx, Al<sub>2</sub>O<sub>3</sub>) || <div class="toccolours mw-collapsible mw-collapsed" style="width:300px> TMA <div class="mw-collapsible-content">trimethylaluminum <br/> (CH<sub>3</sub>)<sub>3</sub>Al <br/> [[File:TMA.png|290px]]</div></div> || style="background-color: #e0b4c6" | No || style="background-color: #c6e0b4" | Yes || [https://doi.org/10.1134/1.1626763]
|-
| Titanium oxide (TiOx, HfO<sub>2</sub>) || <div class="toccolours mw-collapsible mw-collapsed" style="width:300px> TTIP <div class="mw-collapsible-content">Titanium(IV) isopropoxide <br/> (CH<sub>3</sub>)<sub>3</sub>Al <br/> [[File:TTIP.png|290px]]</div></div> || style="background-color: #c6e0b4" | Yes || style="background-color: #e0b4c6" | No || [https://doi.org/10.1134/1.1626763]
|}
|}
== Videos on operating the tools ==
Video on how to operate ALD 1:
[[File:ALD1.mp4|500px]]
* [https://youtu.be/Do91YRRgI34 Click here to watch the video on YouTube]
Video on how to operate ALD 2:
[[File:ALD2.mp4|500px]]
* [https://www.youtube.com/watch?v=GmNEbyMNC4A Click here to watch the video on YouTube]


== Standard operating procedure ==
== Standard operating procedure ==
[https://youtu.be/Do91YRRgI34 Click here to watch our video on operation of ALD 1].
* Log your process in the Excel notebook.
[https://www.youtube.com/watch?v=GmNEbyMNC4A Click here to watch our video on operation of ALD 2]
* Check the nitrogen bottle:
* Open valve on top of the nitrogen bottle.
** Verify that the main valve on top of the bottle is open.
* Check nitrogen bottle pressure. Main bottle pressure should be at least 5 bar, line pressure 3 bar (AJA1) 1-2 bar (AJA2).
*: ''The N2 flow in idle state is '''5 sccm'''.''
*: If line pressure is outside of range, carefully adjust the regulator valve with the flow set to 20 sccm.
** Verify that the main bottle pressure is at least 5 bar.
** The line pressure should be  >1 bar (ALD1) 1-2 bar (ALD2).
*: ''If line pressure is outside the range, please report it to the cleanroom staff.''
* Make sure the valves of '''all''' precursors inside the ALD machine are closed.
* Make sure the valves of '''all''' precursors inside the ALD machine are closed.
* Run recipe ''Default_cleaning'' to pump out any residual gas in the gas lines.
* Run recipe ''Default_cleaning'' to pump out any residual gas in the gas lines.
*: With flow set to 0 the actual flow can be between 0-1 sccm.
* Press the '''VENT''' or '''VENT REACTOR''' button.
* Press the ''VENT'' or ''VENT REACTOR'' button.
* Open the metal lid.
* Open the metal lid.
* Put your sample inside, roughly in the center, away from the gas inlet and outlet.
* Put your sample inside, roughly in the center, away from the gas inlet and outlet.
*: Check whether the rubber O-ring is properly seated.
*: Check whether the rubber O-ring is properly seated.
* Close the metal lid. Check that the lid is aligned to sit directly on top of the reactor chamber.
* Close the metal lid. Check that the lid is aligned to sit directly on top of the reactor chamber.
* Press the big round ''PUMP'' or ''PUMP REACTOR'' button.
* Press the '''PUMP''' or '''PUMP REACTOR''' button.
*: Pressure with flow set to 0: ~5e-2 Torr or lower.
*: Pressure with flow set to 0: ~5e-2 Torr or lower.
* Place the metal cage on top of the tool.
* Place the metal cage on top of the tool.
* Open relevant precursor valves.
* Open relevant precursor valves.
* Run your recipe.
* Run your recipe.
*: Pressure with 20 sccm N<sub>2</sub> flow present: low e-1 Torr.
<blockquote style="background-color: #F0F0F0; border: dashed thin grey;">
*: ALD1 pulse lengths: H<sub>2</sub>O ~0.5 s, HfOx TDMAH 0.2 s, AlOx TMA 0.02 s.
* Pressure with 20 sccm N<sub>2</sub> flow present: low e-1 Torr.
*: ALD2 pulse lengths: H<sub>2</sub>O ~0.02 s, HfOx TDMAH 0.2-0.5 s.
* ALD1 pulse lengths: H<sub>2</sub>O ~0.5 s, HfOx TDMAH 0.2 s, AlOx TMA 0.02 s.
* ALD2 pulse lengths: H<sub>2</sub>O ~0.02 s, HfOx TDMAH 0.2-0.5 s.
</blockquote>
* Close precursor valves.
* Close precursor valves.
* Press the big round ''VENT'' or ''VENT REACTOR'' button.
* Press the big round '''VENT''' or '''VENT REACTOR''' button.
* Place the metal cage on the side of the tool.
* Place the metal cage on the side of the tool.
* Take out your sample. Check the rubber o-ring.
* Take out your sample. Check the rubber o-ring.
* Press the big round ''PUMP'' or ''PUMP REACTOR'' button.
* Press the big round '''PUMP''' or '''PUMP REACTOR''' button.
* Close the nitrogen bottle valve on top of the bottle.
* Run recipe ''Default_heater_set''.
* Run recipe ''Default_heater_set''.
* Verify that the flow is set at 5 sccm.
== Witness samples ==
In CR1 and CR2, you can find various witness samples depending on the properties that you would like to explore:
* Only thickness: Si (001) of dimension > 7x7 mm2
* Thickness and breakdown voltage: Si (001) 15x15 mm2 back-side Au plated
It is recommended to ash the witness chips for 2 mins before loading them in the ALD tool.


== Technical notes ==
== File logs ==


* Recipe file location
* Recipe file location
Line 69: Line 107:
== Troubleshooting ==
== Troubleshooting ==


* Pressure reading obviously wrong (above 1e3 Torr or below 1e-4 Torr):
; Pressure reading obviously wrong (above 1e3 Torr or below 1e-4 Torr):
** Pressure gauge failure. Unplug the network cable from the small square pressure gauge beneath the chamber and plug it back in. The pressure reading should return to expected values.
: Pressure gauge failure. Unplug the network cable from the small square pressure gauge beneath the chamber and plug it back in. The pressure reading should return to expected values.
* No peak visible during precursor pulse:
; No peak visible during precursor pulse:
** Precursor valves closed. Make sure the relevant precursor valves are open. Consult the labels on the inside of the door.
:* Precursor valves closed. Make sure the relevant precursor valves are open. Consult the labels on the inside of the door.
** Pulse time too short. Select the lowest plotting interval and check whether you can spot a small peak when the automatic valve opens. Increase pulse time as needed.
:* Pulse time too short. Select the lowest plotting interval and check whether you can spot a small peak when the automatic valve opens. Increase pulse time as needed.
* Cannot open lid upon venting:
; Cannot open lid upon venting:
** Chamber pressure still below atmosphere. Confirm pressure reading in software. If pressure is below 5e2 Torr, check whether the nitrogen bottle valve is open.
:* Chamber pressure still below atmosphere. Confirm pressure reading in software. If pressure is below 5e2 Torr, check whether the nitrogen bottle valve is open.
** Rubber O-ring can get stuck to the lid. Gently but firmly lift the lid. Reseat the O-ring if needed.
:* Rubber O-ring can get stuck to the lid. Gently but firmly lift the lid. Reseat the O-ring if needed.
; What is the best plot time to graph the process pressure?
: It is recommended to plot only several pulses, for example 30 seconds or 1 minute total plot time. Setting this value to 1 hour during a run can reduce delay precision, because with a 1 hour plot time many data points need to be refreshed, which consumes a lot of processing resources. It is possible to set the plot time to 1 hour to get an overview of pulse heights, but plot times > 5 minutes are not recommended during a run. <ref>Savannah Maintenance Manual</ref>
; What are the recommended heater temperatures?
: These are the recommended temperatures from the manual:
:* Heaters for the trap (#6):150°C
:* Stop valve (#7): 150°C
:* ALD valve oven (#10): 150°C
:* Precursor Manifold: 150°C
:* Reactor heaters (#8 and #9): 100-200°C
:**ALD1 (#8 and #9): 110°C
 
== Remote access ==
* TeamViewer: ALD1, ALD2
* LogMeIn: ALD1 (CR1), ALD2 (CR2)
[[Category:Tools]]
[[Category:Deposition]]
 
 
==References==

Latest revision as of 11:39, 20 May 2025

Cambridge ALD
Picture of Cambridge ALD text
Essentials
Full nameSavannah S100 (gen. 1)
ManufacturerCambridge NanoTech (Veeco)
DescriptionAtomic layer deposition system
LocationCleanroom 1 (03.2.209A)
Cleanroom 2 (03.2.203B)
Responsibility
PrimaryHarry
SecondaryMartin

Two nearly identical Savannah S100-like systems are used for atomic layer deposition of aluminum, hafnium, and titanium oxide.

Other material deposition alternatives at the NBI cleanroom:


Growth per cycle (GPC) monitoring

  • ALD1 HfOx
    ALD1 HfOx
  • ALD1 AlOx
    ALD1 AlOx
  • ALD2 HfOx
    ALD2 HfOx

Available processes

Deposited material Precursor ALD1 ALD2 Ref.
Hafnium oxide (HfOx, HfO2)
TDMAH
tetrakis(dimethylamino)hafnium
[(CH3)2N]4Hf
Yes No [1]
Aluminum oxide (AlOx, Al2O3)
TMA
trimethylaluminum
(CH3)3Al
No Yes [2]
Titanium oxide (TiOx, HfO2)
TTIP
Titanium(IV) isopropoxide
(CH3)3Al
Yes No [3]

Videos on operating the tools

Video on how to operate ALD 1:

Video on how to operate ALD 2:


Standard operating procedure

  • Log your process in the Excel notebook.
  • Check the nitrogen bottle:
    • Verify that the main valve on top of the bottle is open.
    The N2 flow in idle state is 5 sccm.
    • Verify that the main bottle pressure is at least 5 bar.
    • The line pressure should be >1 bar (ALD1) 1-2 bar (ALD2).
    If line pressure is outside the range, please report it to the cleanroom staff.
  • Make sure the valves of all precursors inside the ALD machine are closed.
  • Run recipe Default_cleaning to pump out any residual gas in the gas lines.
  • Press the VENT or VENT REACTOR button.
  • Open the metal lid.
  • Put your sample inside, roughly in the center, away from the gas inlet and outlet.
    Check whether the rubber O-ring is properly seated.
  • Close the metal lid. Check that the lid is aligned to sit directly on top of the reactor chamber.
  • Press the PUMP or PUMP REACTOR button.
    Pressure with flow set to 0: ~5e-2 Torr or lower.
  • Place the metal cage on top of the tool.
  • Open relevant precursor valves.
  • Run your recipe.
  • Pressure with 20 sccm N2 flow present: low e-1 Torr.
  • ALD1 pulse lengths: H2O ~0.5 s, HfOx TDMAH 0.2 s, AlOx TMA 0.02 s.
  • ALD2 pulse lengths: H2O ~0.02 s, HfOx TDMAH 0.2-0.5 s.
  • Close precursor valves.
  • Press the big round VENT or VENT REACTOR button.
  • Place the metal cage on the side of the tool.
  • Take out your sample. Check the rubber o-ring.
  • Press the big round PUMP or PUMP REACTOR button.
  • Run recipe Default_heater_set.
  • Verify that the flow is set at 5 sccm.

Witness samples

In CR1 and CR2, you can find various witness samples depending on the properties that you would like to explore:

  • Only thickness: Si (001) of dimension > 7x7 mm2
  • Thickness and breakdown voltage: Si (001) 15x15 mm2 back-side Au plated

It is recommended to ash the witness chips for 2 mins before loading them in the ALD tool.

File logs

  • Recipe file location
    ALD1: C:\Savannah\Users\Standard\
    ALD2: C:\Cambridge Nanotech\Recipes\
  • Log file location
    ALD1: C:\ALD data. Includes pressure data, screenshot at termination.
    ALD2: C:\Cambridge Nanotech\Log\. Includes pressure and heater temperature data, screenshot at termination, software event logs.

Troubleshooting

Pressure reading obviously wrong (above 1e3 Torr or below 1e-4 Torr)
Pressure gauge failure. Unplug the network cable from the small square pressure gauge beneath the chamber and plug it back in. The pressure reading should return to expected values.
No peak visible during precursor pulse
  • Precursor valves closed. Make sure the relevant precursor valves are open. Consult the labels on the inside of the door.
  • Pulse time too short. Select the lowest plotting interval and check whether you can spot a small peak when the automatic valve opens. Increase pulse time as needed.
Cannot open lid upon venting
  • Chamber pressure still below atmosphere. Confirm pressure reading in software. If pressure is below 5e2 Torr, check whether the nitrogen bottle valve is open.
  • Rubber O-ring can get stuck to the lid. Gently but firmly lift the lid. Reseat the O-ring if needed.
What is the best plot time to graph the process pressure?
It is recommended to plot only several pulses, for example 30 seconds or 1 minute total plot time. Setting this value to 1 hour during a run can reduce delay precision, because with a 1 hour plot time many data points need to be refreshed, which consumes a lot of processing resources. It is possible to set the plot time to 1 hour to get an overview of pulse heights, but plot times > 5 minutes are not recommended during a run. [1]
What are the recommended heater temperatures?
These are the recommended temperatures from the manual:
  • Heaters for the trap (#6):150°C
  • Stop valve (#7): 150°C
  • ALD valve oven (#10): 150°C
  • Precursor Manifold: 150°C
  • Reactor heaters (#8 and #9): 100-200°C
    • ALD1 (#8 and #9): 110°C

Remote access

  • TeamViewer: ALD1, ALD2
  • LogMeIn: ALD1 (CR1), ALD2 (CR2)


References

  1. ↑ Savannah Maintenance Manual
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