EBL Practical Guide
EBL Practical Guide
NanoPatterning Cleanroom
E-Beam Lithography:
A Practical Guide
USER EXPERIENCE
Introduction
Every researcher comes from a unique background with varying degrees of lab experiences.
This practical guide will focus on how to navigate Stanford Nano Shared Facilities:
NanoPatterning Cleanroom. As our name implies, the NanoPatterning Cleanroom (NPC)
revolves around our electron beam lithography capabilities for nanoscale fabrication. Our
facility is proud to provide researchers with all the equipment necessary to create an e-beam
lithography (EBL) process from start to finish. This Practical Guide will inform the user on what
equipment, services and materials NPC provides to our e-beam community to better support
each user’s process development. The NPC staff is a valuable resource to train users and help
tackle each user’s EBL challenges.
Application
Ideally, everything in a process can be optimized. However, users may be more concerned
about one process parameter over another depending on the application. For example,
photonic applications may require smaller beam currents, step sizes or specific tool equipped
with a fixed-beam-moving-stage (FBMS) in order for low edge roughness to prevent signal loss.
Quantum devices may desire sub 10-nm features to align to previous EBL layers and require
more alignment steps and thereby increase tool usage time. A production prototype might be
concerned with minimizing exposure time and prefer higher beam currents and larger writing
fields. Whatever desired application, a researcher may choose to focus on optimizing one
particular aspect. Therefore, consider the application to optimize certain specifications.
Another consideration is what is the final pattern transfer method? The final pattern transfer
will determine what process parameters to choose. Knowing what the smallest and largest
features in your pattern will help determine other parameters of your process like aspect ratios
of a feature to select the resist thickness. The final pattern transfer would determine whether
the resist should be a single layer of etch resistant material or a bi-layer resist stack for better
lift-off profile and the thickness of the layers. The substrate size and material used will
determine how simple or complex the EBL process might be because there is a great different
between a 3 inch silicon wafer versus a 1x1 mm2 sapphire die.
These subjects will be briefly reviewed in the following sections for your consideration.
Fracturing software is capable of manipulating pattern data such as merging separate layers,
removing overlapping layers so as not to overexpose a region, and add positive or negative bias
to grow or shrink a pattern. Furthermore, fracturing software includes advanced features that
are extremely helpful to EBL. Although each of these advanced features can be delved deeper,
a few can be mentioned here. Proximity effect correction (PEC) takes into account the total
energy a resist is exposed to at a particular area and corrects the exposure dose based on
simulated results; edge features would be exposed with higher doses than non-edge features.
Another advanced technique is sleeve and fill where the outline of a large area is exposed using
smaller beam currents and/or step sizes for higher resolution and inner portion of an area is
“filled” with a larger beam. Another example is field position control where adjacent write
fields can be strategically placed so that stitching boundaries can be minimized. Please see
GeniSys BEAMER more examples of fracturing techniques.
GeniSys BEAMER
The NPC provides GeniSys BEAMER for data fracturing. This software operates on a designated
cleanroom computer. Users can log-in to the computer and access their CAD files through USB
or online access. Once the pattern is fractured, the fractured machine readable file can be
transferred through the NPC network to the appropriate EBL system.
SUBSTRATE
Lithography is a temporary process used to transfer a permanent pattern onto a desired
material, the substrate. In semiconductor processing, substrates generally consist of Si, Ge,
GaAs, InP, GaN, etc. As a research facility, various substrates have been processed in the
cleanroom including non-traditional materials like diamond and sapphire.
Not only can materials vary, but the shape and size may also affect your EBL process.
Processing a 3 inch Si wafer is quite different than processing a 1x1 mm2 diamond die. The EBL
systems are equipped with sample holders for a variety of shapes and sizes.
Moreover, the transparency of a material could complicate a process as some EBL tools use
laser height sensing based on a surface reflection to ensure beam focus. If needed, markers on
transparent substrates can be used for height measurements.
Similarly, the conductivity of the substrate is important to avoid charging affects. The electron
beam needs to have a path for the current to travel through and requires for sample materials
to be of a conductive. Insulating materials will cause charging effects resulting in random
exposure patterns because the exposure position cannot be controlled. Non-conductive
samples require a charge dissipation layer to properly expose a pattern so as not to distort the
beam. A conductive layer is needed for insulating materials.
A sample should not outgas, as this would deteriorate vacuum levels because EBL depends on
a high vacuum environment in order to operate. Therefore, no samples that outgas should be
used in EBL.
No matter what the substrate is, the NPC has done its best to accommodate various substrate
materials.
RESIST
Resist Stocking
Many e-beam lithography resists exists in the industry with varying prices and quality. NPC staff
have chosen several industry standard resists to provide to the e-beam lithography users based
on its process capabilities, material quality and economic feasibility. Stocked resists are
provided in the table below along with its respective solvents for further dilution. For more
information regarding each resist, click on the link for its name.
Bringing in Resist
To bring in new resists, use the SNSF-NPC User External Chemical Intake Form. Should the user
decide to bring in their own resist, all bottles must be checked-in with NPC staff, recorded by
NPC staff on Stanford’s ChemTracker inventory software, and labeled appropriately with user
name, Stanford ID, group or company, and contact information. Make sure original chemical
information is legible. Resists not supplied by NPC can be brought in by the user after
consulting with NPC staff. If there is enough user base requests for a new resist, NPC can
evaluate stocking options. The table below includes acceptable resists in the NPC.
MIBK, 6200.04
Allresist GmbH AR-P CSAR 62 Anisole MIBK:IPA, 6200.09
Xylenes 6200.13
MF-312, 2403
Thinner mr-T
MicroChem ma-N MF-319,
1090 2405
351 Developer
The following negative resists are not provided, but acceptable to bring into NPC.
MF-312,
Dow Corning, HSQ
MIBK MF-319,
DisChem HSQ
351 Developer
To dilute to a specific concentration, see the examples below using a scale to measure
by % Solids by weight. Select an amber jar from the desk drawer to the left of the EBL
Resist solvent cabinet. You may choose to do a solvent clean and N2 dry or use the bottle
as is. Zero the bottle on the scale and begin to add the resist. Once the resist is weighed,
calculate the amount of thinner needed. To mix the solution, close the bottle and shake
or a general use stir bar can be found in the general use glassware storage rack.
(𝐴8) 4
Example of % Solids by Weight from 950k PMMA A8 to A4: (𝐴8) + 𝑋 = 8 | X = A-thinner
(𝐸𝐿13) 6
Example of % Solids by Weight from MMA(8.5)MAA EL13 to EL6: (𝐸𝐿13) + 𝑋 = 13 | X = EL-thinner
Example of % Solids by Weight from ma-N 2403 to 2401: Add to 10 g of ma-N 2403 about 16 g
of recommended thinner mr-T 1090.
Example of % Solids by Weight from ma-N 2405 to 2401: Add to 10 g of ma-N 2405 about 26 g
of recommended thinner mr-T 1090.
Spinning Resist
NPC provides a sample preparation area complete with a programmable spinner.
Consumables of plastic pipettes, glass pipettes and bulbs, and syringes, aluminum foil,
cleanroom wipes, swabs are stocked. Acetone, IPA, Methanol, and Remover PG are also
available.
Programmable Spinner
NPC offers access to a Apogee.
Recipe setting “0” is open for user customization. A typical spin coat program contains features
included in the diagram below. Each step is adjusted accordingly with resist characteristics
considering desired thickness, uniformity, viscosity, etc.
This spinner is equipped with varying vacuum chuck sizes capable of spinning from pieces up
to 6 in wafers. For 8 in wafers, please ask NPC staff. For pieces smaller than the provided chuck
sizes, users can mount samples onto a carrier wafer to spin on resist. For mounted samples,
allow a longer bake time to ensure the solvent properly evaporates.
Spin Curves
Common Manufacturer Spin Curves are posted at the spinner bench. Spin curves are helpful
references to estimate the spin speed for a user specified thickness. The best known method
for accurate thickness results is to use Si test wafers to determine your final spin speed. To do
this, estimate a spin speed based on the spin curve and desired thickness. Measure the
thickness using the ellipsometer. Based on the measured thickness, adjust the spin speed
respectively until the desired thickness is obtained. For manufacturer spin curves, see the resist
table above.
Hot Plates
The NPC is complete with several hot plate options for all resist baking needs. Five (5) hot plates
are provided on the sample preparation bench. The hotplates are calibrated by the NPC Staff,
However, it is recommended for each researcher to have their own reference thermometer to
record temperatures specific to their own processes.
A Triple Hot Plate has standard set points of 90°C, 120°C and 150°C. Other temperatures can
also be set. However, the Triple Hot Plate is NOT to be used above 230°C because the Teflon
coating will deteriorate and delaminate. Use only Teflon coated tweezers on these hotplates
to prevent surface scratches.
Two programmable hot plates by Torrey Pines Scientific are also available.
One additional hotplate is available for lift-off processes for heating Remover-PG up to 70°C.
This hotplate is stored above the sample preparation bench. Staff training and approval is
necessary before using a heated lift-off process.
NOTE: Aluminum foil is not recommended as the foil cannot be flattened perfectly and may not
provide even heat distribution. Thick aluminum sheets are provided should the user need
them.
Ellipsometry
The lab is equipped with a Film Sense FS-1 Ellipsometer. The Film Sense FS-1 Multi-Wavelength
Ellipsometer provides fast and reliable thin film measurements. The film thickness of most
transparent thin films from 0 – 1000 nm can be determined. Optical constants, n & k, and other
film properties can also be measured for many samples.
Several commonly used resist parameters are already programmed into the system. Simply
choose the correct model description and measure the resist thickness. New resist models can
also be programmed. Additional training is required and can be found on SNSF’s website.
Profilometry
A profilometer measures the surface profile of a sample. Once a resist coated sample is
exposed and developed, the profilometer can be used to measure the step height of the resist
and substrate surface. This can be used to confirm an ellipsometry measurement.
Our cleanroom has a Dektak XT-S Stylus Profiler that is capable of quickly and accurately
measuring feature heights on a surface. With noise levels approaching 2-3nm it is capable of
resolving step heights as small as 10nm. Variable force and measurement length settings make
measurements possible on a wide range of materials and structures. A magnified video
targeting system permits positioning the needle tip near small surface features. Additional
training is required and can be found on SNSF’s website.
Laser Microscopy
Laser microscopy can assist in creating height profiles after resist is developed. The Keyence
has a Z-axis resolution of 0.5 nm.
The NPC offers a Keyence VK-X Series 3D Laser Scanning Confocal Microscope. The Keyence VK-
X Series 3D Laser Scanning Confocal Microscope provides non-contact, nanometer-level
profile, roughness, and film thickness data on any material. The lateral resolution of the
microscope is 120 nm using the 408 nm Violet laser light. This tool requires special training;
follow these instructions.
Unaligned Write
Most often, the first process layer does not require any alignment. This is simply an EBL
exposure onto a blank substrate. If the experiment only needs one process layer, then an
unaligned write, or free-write, is sufficient. However, if a process requires two or more
lithography processing steps, this would require the use of alignment marks.
Aligned Write
Aligned writes require the use of alignment marks. The alignment marks are fabricated on a
previous step using either photo or e-beam lithography during the initial layer or the
immediately preceding layer. Additionally, once a marker is used for one step, the resist is
exposed and developed so that any fabrication steps would destroy those markers. Please see
the next section on aligning multiple layers. Therefore, using aligned writes require some
forethought of the whole fabrication process. Below are a few tips on setting up aligned writes.
Whether if one layer aligns well to another layer is described as the overlay accuracy. Keep in
mind that the overlay accuracy is only as good as the tool tolerance used to define the markers.
For example, photolithography defined markers have a realistic resolution on the micrometer
scale, whereas EBL defined markers would be accurate to nanometer resolution. Therefore,
using an EBL defined marker would allow subsequent layers to align a few orders of magnitude
better than a photolithography defined marker.
Global Marks
There are different sets of alignment marks needed to teach the tool where to find the markers
and what the markers refer to. The first type of markers are the global marks. The user must
teach the tool the global mark locations in order to orient the whole wafer. These consist of
markers that are along the four edges or corners of the whole sample and allows coarse
alignment and rotation adjustments. Each sample should have at least two global marks, but
four are recommended because two markers would mainly allow one-dimensional
adjustments, while four markers allow x- and y-axis shifts, scaling, skew and rotation
adjustments.
Global marks must be fabricated on a previous step. Global marks can be unique markers used
specifically for global alignment. Or they can also be local markers used during the same write.
The important factor is that the global mark locations are defined for the tool to locate and set
up a coordinate system.
Local/Chip Marks
Just as global marks define the coarse coordinates of the whole sample, local marks define the
fine coordinates of each region. Since the smaller local regions are usually chips, the term chip
marks are used synonymously. Local marks are usually located on the corners of each chip
used to create a chip coordinate system. These locations are also defined by the user for the
tool to set up a coordinate system.
As previously mentioned, multiple aligned writes require multiple sets of markers for each
layer. A few tips to creating new alignment marks are to 1) separate each marker by a distance
of 100um so as not to cross-contaminate, 2) using different marker designs and/or sizes to
distinguish between each set, 3) make the markers at least relatively equidistant to the center
of the chip or if possible, make them closer towards the center than the previous set of markers.
Figure 2: The different contrast levels detected between a marker and the substrate is
demonstrated between a metal (left) and an etched marker (right).
For an etched marker, the depth of etch must be deep enough to cause contrast in the
backscatter detector. Considering that an etch process is a hole of the same material, the
contrast is not based on material but topography. Therefore, etched markers are generally on
the order of microns (~2 µm) rather than nanometers. The NPC is equipped with a reactive ion
etcher (RIE: Oxford PlasmaPro 80). Please see Section: Pattern Transfer.
If the material is a deposited metal, the metal should be a relatively heavier material with high
atomic number than the substrate and thick enough so the electron beam would not penetrate
through the material. For example, 75nm layer of Au or Pt on top of a Si substrate will work for
a 100kV EBL system. The material contrast between the substrate and the marker is large
enough for the backscatter detector to detect a signal. In comparison, 5nm of Au may not work
because a 100kV electron beam would shoot through it and not have enough Au material to
backscatter electrons. The NPC is equipped with a metal evaporator tool (KJL evaporator).
Please see Section: Pattern Transfer.
Cross 50-100 µm 3 µm
Global Marks
Square 5-30 µm 5-30 µm EBPG
Cross 10-50 µm 1-3 µm
Local Marks L 10-50 µm 3 µm
Square 5-30 μm 5-30 μm EBPG
Marker Open
Markers may become covered by additional processes such as oxide layers for isolation that
are not penetrable by the electron beam. Marker opens are large rectangles exposed in resist
during etch steps to remove thick layers of oxide.
Measuring Misalignment
The overlay accuracy between different layers can be measured using traditional verniers in
the X and Y directions. For samples with limited size and real estate, Box-in-Box
measurements may also be added to compare overlay between layers. An example of a Box-
in-Box design is below. Box-in-Box measurements can be analyzed using an SEM.
Training
Each of the EBL systems are from different manufacturers that use different operating
instructions, systems and software. Therefore, each of the systems require separate tool
operations training. Please specify which tool you are interested in using during the new user
EBL Intake Form.
Should any problems arise during a user session, contact the EBL staff. Contact information is
located at the end of this document.
General Information
High Vacuum
In order for the electron beam to function, this requires a high vacuum environment. Make sure
your sample does not outgas. If the sample outgases, the EBL chamber will not be able to pump
down to operating levels. This may cause pump down processes to time out and other adverse
consequences. Additionally, the vacuum environment can be affected if dust, lint, fibers and
other particles enter the EBL loading and main chambers. Preventative measures should be
taken to ensure no particles can contaminate the high vacuum environment. This includes and
is not limited to using a nitrogen gun to blow off the sample and the holder, wearing gloves
over the cleanroom suit cuffs, minimized use of cleanroom wipes in EBL preparation area, and
wearing a face mask covering the mouth.
High Voltage
Each EBL system operates at its respective high voltages. Do not touch any portion of the EBL
column, cables or wires. The emitter material is biased with a high voltage so that electrons
can be extracted from the emitter to form a beam using electromagnetic lenses. In the process,
x-rays are produced, but are contained within the column. Do not attempt to tamper with the
column.
Developer Stocking
Many e-beam resist developers exist in the industry with varying prices and quality. Resist
companies often offer their own brand of developers specific to their resist at a premium. NPC
staff have chosen several industry standard developers to provide to the e-beam lithography
users based on its process capabilities, material quality and economic feasibility. Stocked
developers are provided in the table below along with its respective solvents for dilution. If a
user would like to bring in a new chemical, use the SNSF-NPC User External Chemical Intake
Form.
Wet Benches
Developers come in different forms and concentrations. Depending on the type of resist, users
may require a solvent or aqueous developer. The user must develop their sample in the
corresponding wet benches. NPC has three wet benches for solvents, bases and acids. All users
are required to complete a wet bench training covering safety and operating procedures. If you
require wet bench training, sign up on the training calendar.
Ultrasonic Bath
The Solvent Bench is equipped with a SweepSONIK ultrasonic bath operating at 104 kHz. This
bath may assist in cleaning samples and metal lift-off processes.
Developers
Vendor Name Resist Dilute With Wet Bench
Resist Strippers
Vendor Name Resist Wet Bench
48% Hydrofluoric Acid Acid
HSQ
Buffered Oxide Etch (BOE) 6:1 Acid
PMMA,
Copolymer,
Fisher Scientific Acetone Solvent
ZEP 520A,
ma-N
Methanol Solvent
Rinse
IPA Solvent
PMMA,
Copolymer,
Kayaku Remover PG (NMP) ZEP 520A, Solvent
AR-P CSAR 62,
ma-N
Caution
In theory, all chemicals should be treated with the same respect whether using a common
solvent or a strong acid or base. In reality, constant reminders are needed. Therefore, it is
important to identify two chemicals that have reported fatal injuries.
TMAH is a toxic base. Any exposure to any amount of TMAH can cause injury. In particular, 25%
TMAH has been documented to cause fatal injuries in the following study. Therefore, the staff
highly recommend using alternative developers for user processes. The NPC stocks
comparable developers including MF-312 and MF-319 with lower TMAH concentrations and 351
Developer.
Hydrofluoric Acid (HF) is a strong acid that penetrates the skin and attacks the calcium in the
bone and can lead to fatal injuries. Buffered Oxide Etch (BOE) contains HF.
The mentioned chemicals are not exhaustive of all NPC dangerous chemicals, but those for EBL
processing. Wet bench training must be completed prior to using the wet benches.
INSPECTION
In order to inspect the results of your pattern in resist or final pattern transfer, the NPC offers
several characterization tools.
Optical Microscopy
The NPC has an Olympus microscope with lens magnifications of 5x, 20x, 50x and 100x. The
Dark Field objectives to 20x permits inspection of some nanoscale features not visible in Bright
Field. The microscope is connected to a computer with image capturing software. This
microscope does not require specialized training.
Laser Microscopy
The NPC offers a Keyence VK-X Series 3D Laser Scanning Confocal Microscope. The Keyence VK-
X Series 3D Laser Scanning Confocal Microscope provides non-contact, nanometer-level
profile, roughness, and film thickness data on any material. The lateral resolution of the
microscope is 120 nm using the 408 nm Violet laser light. This tool requires special training;
follow these instructions.
The Nova NanoSEM is complete with a variety of sample holders from pieces up to 4 in wafers.
The stage has a maximum travel range of 110 x 110 mm2 and can be rotated 360° as well as
tilted from -15° to 75°. For greater tilt angles, pre-tilted specimen holders of 45° and 90° can be
mounted.
The NanoSEM is upgraded with a QuickLoader, a smaller load chamber that allows for faster
loading of pieces. This circumvents having to vent the whole SEM chamber in order to load a
substrate saving up to 10 minutes of loading and unloading time. The Nova NanoSEM requires
additional training; please see the following instructions.
PATTERN TRANSFER
Since lithography is only a temporary pattern layer and a means to a goal, it requires a pattern
transfer technique. The NPC is furnished with two main pattern transfer tools: Metallization
and Etch.
Metal
The metal deposition tool in the NPC is manufactured by Kurt J. Lesker Company. It uses an e-
beam evaporation technique. Some key features includes sample sizes from pieces to 6 in
wafers. Stocked materials are Ag, Al, Au, Cr, Cu, Ge, Ni, Pd, Pt, and Ti. For more information
regarding equipment and special training, follow these instructions.
Etch
An equally important pattern transfer method is etching into a material. The NPC operates an
Oxford 80 Reactive Ion Etcher. Key features offered by this equipment include sample sizes of
up to 8 in wafers and a RF generator of 300 W, 13.56 Mhz. Standard etch recipes for silicon and
silicon oxides are readily available. Ar or O plasma recipes can be used for cleaning substrates
and removing resists. There are five different gases plumbed into the chamber: CHF 3, CF4, Ar,
O2, and SF6.
Additional recipes can be created with NPC staff guidance once a user is trained and qualified.
For more information and training, follow these instructions.
MORE INFORMATION
Stanford University is proud to be a part of the National Nanotechnology Coordinated
Infrastructure (NNCI) Network. For more information regarding the NNCI Network, please see
https://www.nnci.net/. Below are a few additional resources that may help you in your
nanofabrication projects.
Stanford
√ nano@stanford https://www.edx.org/course/nano-stanford
University
Duke
√ EBL Intro Video https://www.coursera.org/learn/nanotechnology
University
EBL Class, Slides
UC Berkeley Electron Beam Lithography Class
and Videos
Please suggest additional resources to the email below.
CONTACT INFORMATION
For more information, questions or suggestions, contact the NPC staff:
[email protected].
Staff Charges
If the user requires additional training outside of the standard training session, additional staff
charges will be assessed based on the SNSF Fee Schedule.
Emergencies
For emergencies that would cause harm to a person or the tool, call the NPC Staff at 650-391-
6975.
Version History
Date Editor Change Log
8/7/2019 Stanley Lin Initial Document
8/13/2019 Grant Shao Edited
11/01/2019 Stanley Lin Updated Charge Dissipation and Markers section
11/14/2019 Stanley Lin Updated Resist Stripper section
11/27/2019 Stanley Lin Edited
12/04/2019 Stanley Lin Added Resist Thickness Measurement section
12/06/2019 Stanley Lin Updated Spin Curves
08/07/2020 Stanley Lin Updated Multiple Alignment section
09/14/2020 Stanley Lin Added Dilute Resist section
12/4/2020 Stanley Lin Updated links
2/22/2020 Stanley Lin PMGI and Dilute Resist
1/26/2022 Stanley Lin mr-Conductive Layer
11/11/2022 Stanley Lin Removed JEOL, Nabity, Added DisCharge H2O
04/17/2023 Stanley Lin Updated Xylenes for CSAR, EBPG 5200 Plus,
Removed JEOL
02/01/2024 Stanley Lin Added Box-in-Box measurement
08/20/2024 Stanley Lin Updating links, removed VOYAGER information
If there are sections that you think would help better complete this document, please email
your general suggestions to [email protected].