3M Novec Dry Fluid

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3M™ Novec™ Engineered Fluids

For Vapor Drying of Semiconductor Wafers

Precision
Drying
The nonflammable, “drop-in”
alternative to IPA. Safe for
delicate films and photoresists.
3M™ Novec™ Engineered Fluids

Solvent technology for drying of semiconductor wafers


The Marangoni effect describes the behavior of liquid on the wafer surface resulting from a surface
tension gradient at the gas/liquid interface. This effect results in liquid on the wafer surface being
pulled back into the immersion bath as the wafer is removed from the tank. Because IPA has a much
lower surface tension (22 dynes/cm) than water (73 dynes/cm), when IPA from the vapor dissolves
into the water at the gas/liquid interface, a surface tension gradient is created.
IPA in nitrogen has been the mainstay of wafer drying for nearly 20 years1, 2 but this process has
limitations for advanced semiconductor devices. Due to the low flashpoint of IPA, it is necessary to
limit the amount of IPA in nitrogen to less than 2% to maintain a nonflammable condition. It has also
Marangoni Dry Mechanism been reported3,4 that IPA can remain on a wafer surface after a drying process, leaving a residue
that could form Si-C bonds during a subsequent high temperature process, thereby degrading thin
oxide reliability.
3M™ Novec™ Engineered Fluids offer an alternative to IPA, with physical properties that overcome
current drying limitations. 3M™ Novec™ 7100 and 71IPA Engineered Fluids are both nonflammable
and are compatible with materials of construction in IPA vapor drying systems. Novec fluids have
low water solubility and high vapor pressures that prevent residue formation on surfaces subsequent
to the drying step.
Novec 7100/N2
Spray Mixture
A sustainable, high-performance alternative to IPA
As semiconductor features become smaller, more complex and densely packed, there is growing
concern about the use of aggressive solvents such as IPA in certain applications. Even the slightest
amount of unwanted etching can cause serious defects that increase the chance of device failures
and rejects. Applications such as multilayer photoresists and double patterning of photoresists have
delicate features that are soluble in IPA. The use of solvents such as IPA can lead to critical dimension
changes, adversely impacting device yield. Novec fluids do not etch photoresists.
DI Water Bath Novec 7100 fluid, methoxy-nonafluorobutane (C4F9OCH3), is a clean, colorless and low-odor
fluid with an outstanding balance of safety, performance and environmental characteristics.
A combination of unique physical properties, including low surface tension, low viscosity and high
vapor pressure, makes Novec 7100 fluid ideal for use in surface tension gradient drying. And
Surface tension gradient draws water
away from surface because Novec fluids are nonflammable, they can be used under a wider range of process conditions
compared to IPA, which has flammability limits of 2% in air.
Novec 7100 fluid is low in toxicity. It also has zero ozone depletion potential and low global warming
potential. Because it does not contribute to the formation of photochemical smog, it is exempt from
the definition of a volatile organic compound (VOC).

Structure of Novec 7100 Fluid Typical Physical Properties Environmental and Safety Properties and
Novec Novec Exposure Guidelines
IPA Novec 7100
7100 71IPA
Boiling point (°C) 61 55 82 Exposure Guidelines (ppm) 750
Vapor pressure (torr) 200 207 44 (8 hr. time-weighted average)
Surface tension (dynes/cm) 13.6 14.5 22 Acute LC50, ppm >100,000
Viscosity (cPs) 0.58 .75 2.27 Ozone Depletion Potential (ODP) 0.0
Density (g/ml) 1.52 1.48 0.79 Atmospheric Lifetime, yrs. 4.1
Flashpoint (°C) None None 12 Global Warming Potential (GWP)1 297
F O H C Flammability Limits None None <2%
Hazardous Air Pollutant No
(%) in nitrogen VOC (U.S. EPA definition) No

As shown here, Novec 7100 and Novec 71IPA fluids


1
GWP–100 year integrated time horizon; CO2 = 1.0
(71IPA contains 4.5% w/w IPA) have lower surface For Environmental and Safety Properties and Exposure
tensions compared to IPA but significantly higher Guidelines for Novec 71IPA fluid please contact your
vapor pressures. Because of this and because they 3M technical service representative.
are nonflammable, Novec 7100 and 71IPA fluids
can be run at much broader concentration ranges 3M™ Novec™ 7100 Engineered Fluid has been found
than IPA. to be acceptable as a cleaning and drying solvent by
many major environmental regulatory bodies around
the world. For instance, it is listed by the U.S. EPA as
“Acceptable Without Restrictions.” Novec fluids have
zero ozone-depletion potential, short atmospheric
lifetimes and are low in Global Warming Potential.
Process results Vapor Generation
New research has shown that 3M Novec 7100 Engineered Fluid can address the performance
™ ™

Novec 7100
limitations of IPA in wafer cleaning and drying – and can be used as a virtual drop-in replacement Liquid
for IPA in surface tension gradient drying. Process development has been completed with Novec
7100 and 71IPA fluids. Novec 71IPA fluid is a blend of Novec 7100 fluid (95.5% w/w) and IPA Nitrogen Bubbler MFC
(4.5% w/w).
Concentration
In tests conducted by 3M, particle performance was evaluated using Novec 7100 fluid in a surface Monitor (optional)
tension gradient vapor dryer. 200mm bare silicon wafers were processed in an automated wafer Filter
Process
cleaning immersion system. Wafers were processed with a mixture of ammonium hydroxide, Chamber (optional)
hydrogen peroxide and DI water (SC-1) followed by rinsing in DI water. The wafers were then
dried with Novec 7100 fluid in nitrogen instead of IPA in nitrogen. Wafers defects were measured
prior to and after drying on a KLA Tencor SP2 wafer inspection system, scanning defects with One common method to generate a vapor stream
of drying agent in nitrogen is the bubbler method.
nominal sizes greater than or equal to 45nm. Figures 1 and 2 show the wafer maps before and
A simplified configuration is shown here. In this
after cleaning.
configuration, nitrogen gas is bubbled into liquid
Novec 7100 fluid, resulting in a mixture of Novec
fluid and nitrogen that is then delivered to the
process chamber. The nitrogen flow rate may
be controlled by a mass flow controller (MFC)
and/or a bubbler pressure (BP) regulator. Some
systems offer a nitrogen heater to raise and control
incoming nitrogen temperature.
Nitrogen temperature, nitrogen flow rate and
bubbler pressure are variables for controlling the
final gas concentration. The optional concentration
monitor measures the amount of Novec 7100 fluid
used during a wafer drying sequence.

Figure 1. Pre-scan on SP2 showing Figure 2. Post-scan on SP2 showing


Novec 7100 Concentration (%)
6
BP = Low BP = Medium BP = High
46 total defects. 37 total defects. 5

Converting from IPA to 3M Novec Engineered Fluids


™ ™
3

Specific details will vary depending on the exact cleaning system used. The following 2

are the steps necessary for a general cleaning system: 1

• Remove IPA via purging bubbler with filtered nitrogen 0


0 20 40 60 80 100 120 140 160 170 200
• Fill with Novec fluid and flush with filtered nitrogen Time (sec)
• F ill with Novec fluid Note: BP refers to the bubbler pressure setting
• S ystem ready for testing used to control Novec 7100 fluid in a nitrogen
carrier gas. Increasing the bubbler pressure
Novec 7100/N2 results in a decrease of Novec 7100 fluid in the
Spray Mixture vapor phase.

DI Water Bath
3M™ Novec™ Engineered Fluids

Resources
3M™ Novec™ Engineered Fluids are supported by global sales, technical and customer service
resources, with technical service laboratories in the U.S., Europe, Japan, Taiwan, Korea and
Singapore. Users benefit from 3M’s broad technology base and continuing attention to product
development, performance, safety and environmental issues. For additional technical information
on Novec fluids in the United Sates, or for the name of a local authorized distributor, call 3M
Electronics Markets Materials Division: 800-810-8513.

References
1. A. F. M. Leenaars, J. A. M. Huethorst, J. J. van Oekel, Marangoni Drying: A New Extremely Clean
Drying Process. American Chemical Society, 1990. Volume 6, p. 1701-1703.
2. J. Marra, J. A. M. Huethorst, Physical Principles of Marangoni Drying. American Chemical
Society, 1991. Volume 7, p. 2748-2755.
3. K. Miya, T. Kishimoto, A. Izumi, Non-IPA Wafer Drying Technology for Single-Spin Wet Cleaning.
Electrochemical Society Proceedings, 2003. Volume 26, p. 57-63.
4. K. Motai, T. Itoga, T. Irie, The Effect of Isopropyl Alcohol on the Electrical Characteristics of Thin
Oxide. Japanese Journal of Applied Physics, 1998. Volume 37, p. 1137-1139.

The 3M™ Novec™ The Novec brand is the hallmark for a variety of patented 3M products. Although each has its own unique formula and performance properties, all
Brand Family Novec products are designed in common to address the need for safe, effective, sustainable solutions in industry-specific applications. These include
precision and electronics cleaning, heat transfer, fire protection, lubricant deposition and several specialty chemical applications.
3M™ Novec™ Engineered Fluids 3M™ Novec™ Aerosol Cleaners 3M™ Novec™ 1230 Fire Protection Fluid 3M™ Novec™ Electronic Coatings 3M™ Novec™ Electronic Surfactants
■ ■ ■ ■

United States China Europe Japan Korea Singapore Taiwan


3M Electronics Markets 3M China Ltd. 3M Belgium N.V. Sumitomo 3M Limited 3M Korea Limited 3M Singapore Pte. Ltd. 3M Taiwan Limited
Materials Division 86 21 6275 3535 32 3 250 7521 813 3709 8250 82 2 3771 4114 65 64508888 886 2 2704 9011
800 810 8513

Product Use: All statements, technical information and recommendations contained in this document are based on tests or experience that 3M believes are reliable. However, many
factors beyond 3M’s control can affect the use and performance of a 3M product in a particular application, including conditions under which the product is used and the time and
environmental conditions in which the product is expected to perform. Since these factors are uniquely within the user’s knowledge and control, it is essential that the user evaluate the
3M product to determine whether it is fit for a particular purpose and suitable for the user’s method of application.
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meets the applicable specifications at the time 3M ships the product. Individual products may have additional or different warranties as stated on product literature, package inserts or
product packages. 3M MAKES NO OTHER WARRANTIES, EXPRESS OR IMPLIED, INCLUDING BUT NOT LIMITED TO, ANY IMPLIED WARRANTIES OF MERCHANTABILITY OR FITNESS
FOR A PARTICULAR PURPOSE OR ANY IMPLIED WARRANTY ARISING OUT OF A COURSE OF DEALING, CUSTOM OR USAGE OF TRADE. User is responsible for determining whether the
3M product is fit for a particular purpose and suitable for user’s application. If the 3M product is defective within the warranty period, your exclusive remedy and 3M’s and seller’s sole
obligation will be, at 3M’s option, to replace the product or refund the purchase price.
Limitation Of Liability: Except where prohibited by law, 3M and seller will not be liable for any loss or damage arising from the 3M product, whether direct, indirect, special, incidental,
or consequential regardless of the legal theory asserted, including warranty, contract, negligence or strict liability.

3
Electronics Markets
Materials Division
3M Center, Building 224-3N-11 Please recycle. Printed in USA.
St. Paul, MN 55144-1000 Issued: 5/09 © 3M 2009.
www.3M.com/novec All rights reserved. 6761HB 3M and Novec are trademarks of 3M.
1-800-810-8513 60-5002-0400-7 Used under license by 3M subsidiaries and affiliates.

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