Specific Process Knowledge/Lithography/EBeamLithography/EBLsubstratePrep: Difference between revisions

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=== Resist coating ===
= Resist coating =
An appropriate EBL resist must naturally be applied to the substrate. DTU Nanolab supplies a number of standard resists, please consult the table below. The default positive EBL resist is AR-P 6200.09 (CSAR). CSAR is installed on [[Specific_Process_Knowledge/Lithography/Coaters#Spin Coater: Gamma E-beam and UV|Spin Coater: Gamma E-beam and UV]] for spin coating of 2", 4" and 6" substrates. For other substrate sizes (i.e. chips) or other resists [[Specific_Process_Knowledge/Lithography/Coaters#Manual_Spin_Coaters|Spin Coater: LabSpin 02/03]] have to be used instead. The standard resist bottles are stored in the chemical cupboard in E-4.
An appropriate EBL resist must naturally be applied to the substrate. DTU Nanolab supplies a number of standard resists, please consult the table below. The default positive EBL resist is AR-P 6200.09 (CSAR). CSAR is installed on [[Specific_Process_Knowledge/Lithography/Coaters#Spin Coater: Gamma E-beam and UV|Spin Coater: Gamma E-beam and UV]] for spin coating of 2", 4" and 6" substrates. For other substrate sizes (i.e. chips) or other resists [[Specific_Process_Knowledge/Lithography/Coaters#Manual_Spin_Coaters|Spin Coater: LabSpin 02/03]] have to be used instead. The standard resist bottles are stored in the chemical cupboard in E-4.




Contrary to most UV resist it is in general not advisable to use HMDS priming when coating with EBL resists. There can of course be exceptions to this but we do not recommend HMDS priming when using the DTU Nanolab supplied EBL resists.
We recommend all groups or users to have their own bottle of e-beam resist inside the cleanroom. Please follow the [[Specific Process Knowledge/Lithography/EBeamLithography/ResistBottles|user resist bottles in the cleanroom guide.]]


==DTU Nanolab supplied EBL resists==


We recommend all groups or users to have their own bottle of e-beam resist inside the cleanroom. Please follow the [[Specific Process Knowledge/Lithography/EBeamLithography/ResistBottles|user resist bottles in the cleanroom guide.]]


{|border="1" cellspacing="1" cellpadding="3" style="text-align:left;" width="95%"
{|border="1" cellspacing="1" cellpadding="3" style="text-align:left;" width="95%"
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|'''Technical reports'''
|'''Technical reports'''
|'''Spin Coater'''
|'''Spin Coater'''
|'''Polynomial'''
|'''Thinner'''
|'''Thinner'''
|'''Developer'''
|'''Developer'''
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|[https://www.allresist.com/wp-content/uploads/sites/2/2020/03/AR-P6200_CSAR62english_Allresist_product-information.pdf AR-P 6200 info]  
|[https://www.allresist.com/wp-content/uploads/sites/2/2020/03/AR-P6200_CSAR62english_Allresist_product-information.pdf AR-P 6200 info]  
|[[Specific_Process_Knowledge/Lithography/Coaters#Spin Coater: Gamma E-beam and UV|Spin Coater: Gamma E-beam and UV]] or [[Specific_Process_Knowledge/Lithography/Coaters#Manual_Spin_Coaters|Spin Coater: LabSpin 02/03]]
|[[Specific_Process_Knowledge/Lithography/Coaters#Spin Coater: Gamma E-beam and UV|Spin Coater: Gamma E-beam and UV]] or [[Specific_Process_Knowledge/Lithography/Coaters#Manual_Spin_Coaters|Spin Coater: LabSpin 02/03]]
|a = 7252.2, b = -0.454
|Anisole
|Anisole
|
|
*AR-600-546
ZED N50
*AR-600-548
*N50  
*MIBK:IPA
|IPA
|IPA
|
|
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|[https://www.allresist.com/wp-content/uploads/sites/2/2020/03/SXAR-N8200-1_english_Allresist_product_information.pdf AR-N 8200 info]
|[https://www.allresist.com/wp-content/uploads/sites/2/2020/03/SXAR-N8200-1_english_Allresist_product_information.pdf AR-N 8200 info]
|[[Specific_Process_Knowledge/Lithography/Coaters#Manual_Spin_Coaters|Spin Coater: LabSpin 02/03]]
|[[Specific_Process_Knowledge/Lithography/Coaters#Manual_Spin_Coaters|Spin Coater: LabSpin 02/03]]
|a = ?, b = ?
|AR 600-07
|AR 600-07
|AR 300-47:DIW (1:1)
|AR 300-47:DIW (1:1)
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|-
|-
|-style="background:LightGrey; color:black"
|-style="background:WhiteSmoke; color:black"
|'''[[Specific_Process_Knowledge/Lithography/ARN7500|AR-N 7500]]'''
|'''AR-N 7520'''
|Negative
|Negative
|[http://www.allresist.com AllResist]
|[http://www.allresist.com AllResist]
|[https://www.allresist.com/wp-content/uploads/sites/2/2020/03/AR-N7500_english_Allresist_product-information.pdf AR-N 7500 info]
|[[media:AR-N7500-7520.pdf‎|AR-N7500-7520]]
|[[Specific_Process_Knowledge/Lithography/Coaters#Manual_Spin_Coaters|Spin Coater: LabSpin 02/03]]
|[[Specific_Process_Knowledge/Lithography/Coaters#Manual_Spin_Coaters|Spin Coater: LabSpin 02/03]]
|a = 17126, b = -0.435
|PGMEA
|PGMEA
|
|
*AR 300-47:DIW (4:1)
*AR 300-47  
*MIF726:DIW (8:5)
*MIF 726
|DIW
|H2O
|
|
*AR 300-73
*O2 plasma
|
|


|}
|-
|-style="background:LightGrey; color:black"
|'''[[Specific Process Knowledge/Lithography/EBeamLithography/AR-P 617|AR-P 617]]'''
|Positive
|[http://www.allresist.com AllResist]
|[https://www.allresist.com/wp-content/uploads/sites/2/2020/03/AR-P610_english_Allresist_product-information.pdf AR-P 617 info]
|[[Specific_Process_Knowledge/Lithography/Coaters#Manual_Spin_Coaters|Spin Coater: LabSpin 02/03]]
|PGMEA
|AR 600-50
|IPA
|Remover 1165
|


Resist thickness as function of spin speed on Lab Spin 2/3 can be estimated from the parameters above as y = ax<sup>b</sup>, where y is resist thickness in nm and x is spin speed in RPM.
|-
|-style="background:WhiteSmoke; color:black"
|'''[[Specific Process Knowledge/Lithography/EBeamLithography/ma-N 2400|ma-N 2400]]'''
|Negative
|[https://www.microresist.de/en/produkt/ma-n-2400-series/ Micro Resist Technology]
|
|[[Specific_Process_Knowledge/Lithography/Coaters#Manual_Spin_Coaters|Spin Coater: LabSpin 02/03]]
|Anisole
|
*MIF 726
*ma-D 525
|H2O
|mr-Rem 700
|


|}


==User supplied resists==
It is possible to obtain permission to user other resists at DTU Nanolab, users must however provide these resists and possibly developers themselves. A non-exhaustive list of user supplied EBL resist used at DTU Nanolab and some process guidelines can be found in the table below.
It is possible to obtain permission to user other resists at DTU Nanolab, users must however provide these resists and possibly developers themselves. A non-exhaustive list of user supplied EBL resist used at DTU Nanolab and some process guidelines can be found in the table below.


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|-
|-
|-style="background:LightGrey; color:black"
|-style="background:LightGrey; color:black"
|'''AR-N 7520'''
|'''[[Specific_Process_Knowledge/Lithography/ARN7500|AR-N 7500]]'''
|Negative
|Negative
|[http://www.allresist.com AllResist]
|[http://www.allresist.com AllResist]
|Both e-beam, DUV and UV-sensitive resist. Currently being tested, contact [mailto:pxshi@dtu.dk Peixiong Shi] for information.
|[https://www.allresist.com/wp-content/uploads/sites/2/2020/03/AR-N7500_english_Allresist_product-information.pdf AR-N 7500 info]
|[[media:AR-N7500-7520.pdf‎|AR-N7500-7520]]
|[[Specific_Process_Knowledge/Lithography/Coaters#Manual_Spin_Coaters|Spin Coater: LabSpin 02/03]]
|See table <u>[[Specific_Process_Knowledge/Lithography/Coaters#Coaters:_Comparison_Table|here]] </u>
|a = 17126, b = -0.435
|PGMEA
|PGMEA
|AR 300-47, TMAH
|H2O
|
|
*AR 300-47:DIW (4:1)
*MIF726:DIW (8:5)
|DIW
|
*AR 300-73
*O2 plasma
|
|


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<br/>
<br/>


=== Discharge layer application ===
==Current EBL resist stock==
As exposure is done with an electron beam, insulating substrates will cause a build up of charge that will deflect the incoming beam and disturb pattern definition. It is therefore necesarry when working with insulating substrates or substrates with thick (> 200 nm) dielectric films to apply a discharge layer. This is typically applied on top of the EBL resist layer and must be removed in between exposure and development. The most common discharge layer is 20 nm thermally evaporated Al. Bear in mind that it should be thermally evaporated and not e-beam evaporated. Thermal evaporation of Al can be done in [[Specific_Process_Knowledge/Thin film deposition/thermalevaporator|Thermal evaporator]] and [[Specific_Process_Knowledge/Thin film deposition/Wordentec|Wordentec]]. The Al layer can be removed with MIF726 after exposure. MIF726 etch rate in Al is about 0.5 nm/s, although only about 1 nm/min in oxidized aluminium.
The table below indicates the current stock of Nanolab provided EBL resists in the resist cupboard in E4.
 
{|border="1" cellspacing="1" cellpadding="3" style="text-align:left;" width="800px"
|-
 
!colspan="4" border="none" style="background:silver; color:black;" align="center"|Current EBL resist stock in E4 (updated 2023-09-04)
|-
 
|-
|-style="background:silver; color:black"
|'''Resist'''
|'''Bottle size'''
|'''Expiration'''
|'''Approximate amount remaining [L]'''
 
|-
|-style="background:LightGrey; color:black"
|AR-P 6200.09
| 1 L
| 2026
| 1
 
|-
|-style="background:WhiteSmoke; color:black"
|AR-P 6200.04
| 1 L
| 2026
| 1
 
|-
|-style="background:LightGrey; color:black"
|AR-P 6200.04
| 0.25 L
| 2019
| 0.25
 
|-
|-style="background:WhiteSmoke; color:black"
|AR-P 6200.04
| 0.25 L
| 2019
| 0.1
 
|-
|-style="background:LightGrey; color:black"
|AR-N 7520.07 New
| 1 L
| 2018
| 0.8
 
|-
|-style="background:WhiteSmoke; color:black"
|AR-N 7520.11 New
| 0.25 L
| 2024
| 0.25
 
|-
|-style="background:LightGrey; color:black"
|AR-N 7520.17 New
| 0.25 L
| 2026
| 0.25
 
|-
|-style="background:WhiteSmoke; color:black"
|AR-N 7520.18
| 1 L
| 2016
| 0.7
 
|-
|-style="background:LightGrey; color:black"
|AR-N 8200.06
| 0.1 L
| 2021
| 0.1
 
|-
|-style="background:WhiteSmoke; color:black"
|AR-N 8200.03
| 0.25 L
| 2023
| 0.25


For samples with 2D materials such as graphene, HBN, etc., it is '''mandatory''' to apply a 20 nm Al layer on top of the resist in order to expose the substrate in the JEOL 9500 system. The Raith eLine system does not have this requirement.
|}


Another possibility is to use a spin-on conductive layer such as [https://www.allresist.com/wp-content/uploads/sites/2/2021/05/Allresist_Product-information-Protective-Coating-AR-PC-5090_5091-English-web.pdf AR-PC 5090]. It can be removed with water after exposure. At the moment we do not have much experience with this, contact the EBL team if you are interested in this option.
<br clear="all" />


=== Inspection ===
== Discharge layer application ==
As exposure is done with an electron beam, insulating substrates will cause a build up of charge that will deflect the incoming beam and disturb pattern definition. It is therefore necesarry when working with insulating substrates or substrates with thick (> 200 nm) dielectric films to apply a discharge layer. This is typically applied on top of the EBL resist layer and must be removed in between exposure and development. The most common discharge layer is 20 nm thermally evaporated Al. Bear in mind that it should be thermally evaporated and not e-beam evaporated. Thermal evaporation of Al can be done in [[Specific_Process_Knowledge/Thin film deposition/thermalevaporator|Thermal evaporator]] and [[Specific_Process_Knowledge/Thin film deposition/Wordentec|Wordentec]]. The Al layer can be removed with MIF726 after exposure. MIF726 etch rate in Al is about 0.5 nm/s, although only about 1 nm/min in oxidized aluminium.


[[Image:RejectedSamples.png|500x500px|right|thumb|Example of rejected samples with visible bubbles in resist/Al coating and (a lot) of resist residue on the backside.]]
For samples with 2D materials such as graphene, HBN, etc., it is '''mandatory''' to apply a 20 nm Al layer on top of the resist in order to expose the substrate in the JEOL 9500 system. The Raith eLine system does not have this requirement.


== Inspection ==
Post exposure pattern dimensions are dependent on resist thickness. Thus, it is advisable to verify resist thickness after spin coating. This can be done by ellipsometry in the [[Specific_Process_Knowledge/Characterization/Optical_characterization#Ellipsometer|VASE Ellipsometer]].
Post exposure pattern dimensions are dependent on resist thickness. Thus, it is advisable to verify resist thickness after spin coating. This can be done by ellipsometry in the [[Specific_Process_Knowledge/Characterization/Optical_characterization#Ellipsometer|VASE Ellipsometer]].


Line 233: Line 339:


'''Samples with resist residues on the backside will also be rejected.''' If you have resist residues on the backside of your wafer you should wipe it off with an appropriate solvent.
'''Samples with resist residues on the backside will also be rejected.''' If you have resist residues on the backside of your wafer you should wipe it off with an appropriate solvent.
{| style="border: none; border-spacing: 0; margin: 1em auto; text-align: center;"
|-
| [[image:RejectedSamples.png|600px]]
|-
| colspan="1" style="text-align:center;|
Example of rejected samples with visible bubbles in resist/Al coating and (a lot) of resist residue on the backside. Photo: Thomas Pedersen.
|}


<br clear="all" />
<br clear="all" />

Latest revision as of 10:49, 31 May 2024

Resist coating

An appropriate EBL resist must naturally be applied to the substrate. DTU Nanolab supplies a number of standard resists, please consult the table below. The default positive EBL resist is AR-P 6200.09 (CSAR). CSAR is installed on Spin Coater: Gamma E-beam and UV for spin coating of 2", 4" and 6" substrates. For other substrate sizes (i.e. chips) or other resists Spin Coater: LabSpin 02/03 have to be used instead. The standard resist bottles are stored in the chemical cupboard in E-4.


We recommend all groups or users to have their own bottle of e-beam resist inside the cleanroom. Please follow the user resist bottles in the cleanroom guide.

DTU Nanolab supplied EBL resists

DTU Nanolab supplied standard EBL resists and process guides
Resist Polarity Manufacturer Technical reports Spin Coater Thinner Developer Rinse Remover Process flows (in docx-format)
CSAR AR-P 6200 Positive AllResist AR-P 6200 info Spin Coater: Gamma E-beam and UV or Spin Coater: LabSpin 02/03 Anisole

ZED N50

IPA
  • AR-600-71
  • Remover 1165
CSAR
CSAR with Al
LOR5A with CSAR
Medusa AR-N 8200 Negative AllResist AR-N 8200 info Spin Coater: LabSpin 02/03 AR 600-07 AR 300-47:DIW (1:1) DIW BOE
AR-N 7520 Negative AllResist AR-N7500-7520 Spin Coater: LabSpin 02/03 PGMEA
  • AR 300-47
  • MIF 726
H2O
AR-P 617 Positive AllResist AR-P 617 info Spin Coater: LabSpin 02/03 PGMEA AR 600-50 IPA Remover 1165
ma-N 2400 Negative Micro Resist Technology Spin Coater: LabSpin 02/03 Anisole
  • MIF 726
  • ma-D 525
H2O mr-Rem 700

User supplied resists

It is possible to obtain permission to user other resists at DTU Nanolab, users must however provide these resists and possibly developers themselves. A non-exhaustive list of user supplied EBL resist used at DTU Nanolab and some process guidelines can be found in the table below.


Non standard, user supplied EBL resists and process guides
Resist Polarity Manufacturer Comments Technical reports Spin Coater Thinner Developer Rinse Remover Process flows (in docx-format)
ZEP520A Positive resist, contact Lithography if you plan to use this resist ZEON Positive resist ZEP520A.pdf, ZEP520A spin curves on SSE Spinner See table here Anisole ZED-N50/Hexyl Acetate,n-amyl acetate, oxylene. JJAP-51-06FC05‎, JVB001037 IPA acetone/1165 Process Flow ZEP


Copolymer AR-P 617 Positive AllResist Approved, not tested yet. Used for trilayer (PE-free) resist-stack or double-layer lift-off resist stack. Please contact Lithography for information. AR_P617 See table here PGME AR 600-55, MIBK:IPA acetone/1165 Trilayer stack: Process Flow
mr EBL 6000.1 Negative MicroResist Standard negative resist mrEBL6000 processing Guidelines‎ See table here Anisole mr DEV IPA mr REM Process Flow‎
HSQ (XR-1541) Negative DOW Corning Approved. Standard negative resist HSQ Dow Corning, MSDS HSQ See table here TMAH, AZ400K:H2O H2O process flow HSQ

High resolution patterning with HSQ

AR-N 7500 Negative AllResist AR-N 7500 info Spin Coater: LabSpin 02/03 a = 17126, b = -0.435 PGMEA
  • AR 300-47:DIW (4:1)
  • MIF726:DIW (8:5)
DIW
  • AR 300-73
  • O2 plasma
PMMA Positive AllResist See table here Anisole MIBK:IPA (1:3), IPA:H2O IPA acetone/1165/Pirahna


ZEP7000 Positive ZEON Not approved. Low dose to clear, can be used for trilayer (PEC-free) resist-stack. Please contact Lithography for information. ZEP7000.pdf See table here Anisole ZED-500/Hexyl Acetate,n-amyl acetate, oxylene. IPA acetone/1165 Trilayer stack: Process Flow‎


Current EBL resist stock

The table below indicates the current stock of Nanolab provided EBL resists in the resist cupboard in E4.

Current EBL resist stock in E4 (updated 2023-09-04)
Resist Bottle size Expiration Approximate amount remaining [L]
AR-P 6200.09 1 L 2026 1
AR-P 6200.04 1 L 2026 1
AR-P 6200.04 0.25 L 2019 0.25
AR-P 6200.04 0.25 L 2019 0.1
AR-N 7520.07 New 1 L 2018 0.8
AR-N 7520.11 New 0.25 L 2024 0.25
AR-N 7520.17 New 0.25 L 2026 0.25
AR-N 7520.18 1 L 2016 0.7
AR-N 8200.06 0.1 L 2021 0.1
AR-N 8200.03 0.25 L 2023 0.25


Discharge layer application

As exposure is done with an electron beam, insulating substrates will cause a build up of charge that will deflect the incoming beam and disturb pattern definition. It is therefore necesarry when working with insulating substrates or substrates with thick (> 200 nm) dielectric films to apply a discharge layer. This is typically applied on top of the EBL resist layer and must be removed in between exposure and development. The most common discharge layer is 20 nm thermally evaporated Al. Bear in mind that it should be thermally evaporated and not e-beam evaporated. Thermal evaporation of Al can be done in Thermal evaporator and Wordentec. The Al layer can be removed with MIF726 after exposure. MIF726 etch rate in Al is about 0.5 nm/s, although only about 1 nm/min in oxidized aluminium.

For samples with 2D materials such as graphene, HBN, etc., it is mandatory to apply a 20 nm Al layer on top of the resist in order to expose the substrate in the JEOL 9500 system. The Raith eLine system does not have this requirement.

Inspection

Post exposure pattern dimensions are dependent on resist thickness. Thus, it is advisable to verify resist thickness after spin coating. This can be done by ellipsometry in the VASE Ellipsometer.

As the cleanliness requirement of the JEOL is very high, substrates that does not visually appear to be in a good condition will be rejected by the JEOL 9500 cassette loading team. It is therefore a good idea to perform your own visual inspection. The loading team will inspect your samples for any types of flakes or bubbles in the surface layers of the sample. Samples with flakes or bubbles will be rejected.

Samples with resist residues on the backside will also be rejected. If you have resist residues on the backside of your wafer you should wipe it off with an appropriate solvent.


Example of rejected samples with visible bubbles in resist/Al coating and (a lot) of resist residue on the backside. Photo: Thomas Pedersen.