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SEMI P8-0997 © SE MI 1984, 1997 2 4.2.4 Wipe th e needle with lint-free t i ss ue. 4.2.5 Weig h the syringe assembly to t he nearest 0.1 mg (W 3 ). 4.2.6 In j ect the sample into the titrat i o n vessel. 4.2.7 Titrat e t…

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SEMI P8-0997 © SEMI 1984, 19971
SEMI P8-0997
METHOD FOR THE DETERMINATION OF WATER IN PHOTORESIST
1 Scope
1.1 This method is intended for the application of the
Karl Fischer titration to the determination of water in
photoresists. An electrometric method is used for
determining the endpoint. The procedure is applicable
to most resists that have polymer and solvent systems
fully compatible with Karl Fischer reagent and diluent.
The resist manufacturer should be consulted to
determine if this procedure can be used with the resist
in question.
2 Referenced Documents
2.1 ASTM Standard
1
E 203 — Water by the Karl Fischer Method
2.2 Reagent Chemicals — Sixth E dition, American
Chemical Society Specifications
3 Apparatus
3.1 Automatic titrator, equipped for Karl Fischer
titrations. The titrator should be equipped with a
titration vessel with a port for sample entry, desiccated
vent tube, and a platinum versus platinum electrode.
Mechanical stirring of the titration solvent should be
provided for. The manufacturer’s suggested operating
procedure should be followed, and the endpoint timer
set for 20 seconds.
3.2 Hypodermic syringes with lock tip, 0.25 mL and
10 mL.
3.3 Syringe needles, 5 to 8 cm length, 20 and 22
gauge.
3.4 Lint-free tissue.
3.5 Analytical balance, capable of weighing to 0.1 mg.
3.6 Reagents
3.6.1 Distilled water.
3.6.2 Methanol, ACS Reagent Grade.
3.6.3 Karl Fischer reagent with a titer of 3.0 (± 5.0)
mg of water per ml of titrant. Typical preparation
involves a one-to-one dilution of stabilized Karl Fischer
reagent with Karl Fischer diluent from the same
supplier.
1 American Society for Testing and Materials, 100 Barr Harbor
Drive, West Conshohoken, PA 19428-2959
4 Procedure
4.1 Standardization of Karl Fischer Reagent — The
Karl Fischer reagent should be standardized
immediately before its use in water determinations.
4.1.1 Install Karl Fischer reagent in the titrator and
flush all lines of the titration equipment at least three
times.
4.1.2 Fill the titration vessel with enough methanol to
cover the electrodes, and seal.
4.1.3 Titrate the methanol automatically with the Karl
Fischer reagent to the endpoint (blank).
4.1.4 Draw 0.1 mL of distilled water into a 0.25 mL
syringe equipped with a 22 gauge needle. Draw the
water from the needle into the syringe by inverting the
syringe (needle up) and drawing the plunger downward
an additional 1 to 2 cm.
4.1.5 Wipe the needle with lint-free tissue.
4.1.6 Weigh the syringe assembly to the nearest 0.1
mg (W
1
).
4.1.7 Inject the water into the titration vessel.
4.1.8 Titrate to the same endpoint used for the
methanol blank.
4.1.9 Reweigh the syringe assembly to the nearest 0.1
mg (W
2
).
4.1.10 Record the number of milliliters of titrant
consumed (V
1
).
4.1.11 Calculate the Karl Fischer factor (F):
F =
mg water injecte
d
mL KF titrant
=
W
1
−
W
2
V
1
4.1.12
Repeat the standardizing titration twice and
calculate the mean value for F from the three values
(which should fall within a range of 0.02).
4.2
Determination of Water
4.2.1 Fill the titration vessel with enough methanol to
cover the electrodes, and seal.
4.2.2 Titrate the methanol automatically with the Karl
Fischer reagent to the endpoint (blank).
4.2.3 Flush a dry 10 mL syringe fitted with a 20 gauge
needle several times with the sample to be tested. Fill
the syringe with 3–5 mL of photoresist sample.
SEMI P8-0997 © SEMI 1984, 1997 2
4.2.4 Wipe the needle with lint-free tissue.
4.2.5 Weigh the syringe assembly to the nearest 0.1
mg (W
3
).
4.2.6 Inject the sample into the titration vessel.
4.2.7
Titrate to the same endpoint used for the
methanol blank.
4.2.8 Reweigh the syringe assembly to the nearest 0.1
mg (W
4
).
4.2.9 Record the number of milliliters of titrant used
(V
2
).
4.2.10
Calculate the water content of the sample.
Weight % H
2
O=
mL KF titrant × F
sample weight in mg
×100
=
V
2
× F
W
3
− W
4
×100
4.3 Remarks — Photoresists which contain interfering
compounds (such as aldehydes and ketones) may
require modification of the solvent or titration
conditions. For further information, see Section 3.4 of
ASTM Standard E 203. For some negative
(polyisoprene) photoresists, solubility can be improved
by substituting ethylene glycol as the solvent for
methanol.
NOTICE: These standards do not purport to address
safety issues, if any, associated with their use. It is the
responsibility of the user of these standards to establish
appropriate safety and health practices and determine
the applicability of regulatory limitations prior to use.
SEMI makes no warranties or representations as to the
suitability of the standards set forth herein for any
particular application. The determination of the
suitability of the standard is solely the responsibility of
the user. Users are cautioned to refer to manufacturer’s
instructions, product labels, product data sheets, and
other relevant literature respecting any materials
mentioned herein. These standards are subject to
change without notice.
The user’s attention is called to the possibility that
compliance with this standard may require use of
copyrighted material or of an invention covered by
patent rights. By publication of this standard, SEMI
takes no position respecting the validity of any patent
rights or copyrights asserted in connection with any
item mentioned in this standard. Users of this standard
are expressly advised that determination of any such
patent rights or copyrights, and the risk of infringement
of such rights, are entirely their own responsibility.
Copyright by SEMI® (Semiconductor Equipment and Materials
International), 3081 Zanker Road, San Jose, CA 95134. Reproduction o
f
the contents in whole or in part is forbidden without express written
consent of SEMI.
SEMI P9-0298 © SEMI 1988, 19981
SEMI P9-0298
GUIDELINE FOR FUNCTIONAL TESTING OF MICROELECTRONIC
RESISTS
1 Purpose
The purpose of this guideline is to provide a baseline
program of test procedures needed to functionally test
liquid-developed resists, resist developers, and rinses
for microelectronic applications. It can also be used as a
guide to evaluate process modifications to such
systems. This guideline is intended to be applicable for
photo, DUV, x-ray, and electron beam processes.
2 Background
Release of the information in this document was
approved by the SEMI Photolithographic Chemicals
Committee (Resist Committee) in May 1987. This
committee plans to complete and revise the guideline as
appropriate. Comments will be welcomed.
3 Scope
Virtually all lithographic fabrication processes vary in
some way from location to location, even for the same
type of resist. Consequently, it is impossible to provide
a stringent evaluation program acceptable to most users.
It is, therefore, the aim of this guideline to provide a
program of tests and methods that allows variable, but
controlled, process differences. In order to maintain a
proper baseline control for each process, all tests should
be run relative to some internal standard product whose
functional characteristics are known and characterized.
It is understood that each product is to be run at its own
preferred or recommended conditions and that different
products maybe evaluated under different conditions. It
should also be understood that some properties,
variables, or conditions, such as normality, are specific
to resist type, such as positive photoresist, and are to be
used only where applicable. Further, since this guide is
directed to functional testing, it is assumed that any
products to be evaluated have passed all relevant
chemical and physical testing before such functional
testing.
4 Priorities
This guideline has been divided into two separate
groups. The first group, called “Sustaining Tests,”
includes tests that are necessary for timely adjustments
to coating and exposure conditions in order to maintain
consistent image dimensions (Tables 1–3). The second
group, called “Extended Testing,” includes tests that are
required for full evaluation of the resist system (Tables
4–6). These tests may, or may not, be necessary for
evaluation of each lot of product, depending on the
individual requirements of the user.
5 Referenced Documents
5.1 ASTM Standards
1
F 518 — Practice for Determining Effective Adhesion
for Photoresist of Hard-Surface Photomask Blanks and
Semiconductor Wafers during Etching
F 527 — Practice for Adjusting Photoresist Exposure
Time
F 528 — Method for Measurement of Common-
Emmiter D-C Current Gain of Junction Transistors
F 804 — Practice for Producing Spin Coating Resist
Thickness Curves
F 863 — Practice for Detection of Defects in Spin-
coated Resist
F 890 — Practice for Determining Pinhole Density in
Photoresist Films Used in Microelectonics Device
Processsing
F 1059 — Standard Practice for Calculating the
Contrast and Threshold Sensitivity of a Positive
Photoresist
6 Terminology
6.1 test method — A definitive procedure for the
identification, measurement, and evaluation of one or
more qualities, characteristics, or properties of a
material, product, system, or service that produces a test
result.
1 American Society for Testing and Materials, 100 Barr Harbor
Drive, West Conshohoken, PA 19428-2959